thundercles
08-13-2005, 10:42 PM
Disclaimer: I have never EEEEVVVER attempted any of the following processes, that would be illegal, and I'm on the straight and narrow now. Nor do I ever plan to. This is all just the result of a ton of research I have conducted in my spare time for my own intrests that I am now presenting to you for your own educational purposes. I am in no way responsible for what you do with this information, nor do I really care what you do with it.
There are many many ways to make X, the most popular are either via the ketone MDP-2-P or B-Nitropropenes. The most important part is obtaining a precursor chemical, which can be one of three chemicals, all are heavily watched so you have to be crafty to get ahold of them. The three chemicals are Safrole, Isosafrole, and Piperinol. I will start out with some ways to obtain them.
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The easiest way to obtain a precursor chemical is to find some kind of oil or substance already containing a percentage of the chemical in it already and isolating it.
The most common way of getting safrole is via sassafras oil. There are two kinds of this, the American kind and the Brazillian kind. The American kind contains about 80% safrole and the Brazillian about 90-95% (the Brazillian kind can obviously be used as is with no further purification, since it is already almost pure safrole). This oil can be obtained from health food stores or through fragrance or perfume supply companies. Be very careful when purchasing as it is well known what this is used for; it is best to have someone who isn't you buy it for you, especially in any kind of quantity. Other oils containing safrole in about the 40-50% are camphor oil, artificial sassafras oil, and betel leaf oil. Smaller amounts can be found in the oils of cinnamon, mace, and nutmeg. If you live in the eastern US along the eastern seaboard or the Appalachian mountain regions you can actually find the sassafras tree and the trunk and root bark of older, mature trees can be steam distilled to produce safrole. Safrole's boiling point is 234 degrees C at 1atm so get distillin'.
Or you could really luck out and be from Georgia or Florida and have a great plant called the yellow anisetree grow natively in thier area. This tree is a shrub that grows in the low woods and swamps throughout the coastal plains from Florida to Georgia. The oil from its leaves is more than 90% safrole and can be used as is once extracted from the leaves of a plant.
Isosafrole does not occur in nature and can only be manufactured from safrole. It is pretty much interchangeable with safrole as a precursor chemical so we will skip it.
One good idea, even when dealing with the almost pure safrole oils that was forgotten is that you should try and get rid of any eugenol contaminating the oil, as it reacts similar to safrole. To do this simply put the oil in a PP container and stir with an equal amount of 3-5% sodium hydroxide solution. Little white crystals of eugenol anion will form in the water layer. The water layer is poured off and saved (Eugenol can be useful). Wash the oil 3 times while being stirred, then place in a cooking pot and boil at 100 degrees C for a few minutes to boil off all the water.
I dun remember what has piperinol in it except pepper. But it is a bitch to isolate from the pepper and yeilds are low apperently so just try and go for safrole, since to use this guide you will have to make piperinol into safrole anyways. If you do end up with piperinol somehow, try substituting it for benzaldehyde in my speed making technique in the "grand post for all D&B" it should work and could possibly make more potent X theoretically. Of course I've never done any of this shit IRL, I've just read a lot up on it all so I'm interested in knowing how it works, message me if you ever try it. :shifty:
If you were able to use any of the above methods to obtain pure or mostly pure safrole, isosafrole, or piperinol, you can skip to section 3. Otherwise you gotta wade through section two directly below. Don't worry if I were to ever make X I'd have to make my precursors too since I'm too paranoid to go out and buy sassafras oil and I don't live anywhere near sassafras trees or Yellow Anisetrees, the closest wild one of either to me is probably 2000 miles away or so. I also wont go to a nursery and buy a tree to mutalate to make X cause I kind of have a thing against mutalating my own plants, even for drugs. Even though as you all know I have no problem ripping off wild cactus or cactus belonging to other people in thier yards for drugs :D
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At last, if you can't get precursors any of the ways above, you gotta make them from scratch and this is a bitch, and dangerous(actually I think I left the dangerous process out for now, but I'm gonna add it later methinks, so beee careful). It is recommended you have some labrotory experience before ever attempting any of this because, yeah some steps are dangerous.
Basically you start with pyrocatechol, this chemical is common and not watched and should be no problem to get. If it is a problem to get and you can get Salicyladehyde or Guaiacol instead, you can make pyrocatechol out of it, but I don't want to waste my time explaining this if I don't have to, so if this happens to be your case message me or reply stating the situation and I will add this process, otherwise I'll just assume you can get the catechol.
pyrocatechol is a benzene ring with alcohol molecules on two adjacent carbons. The goal of this process is to connect them into a methylenedioxy ring and form 1,3-benzodioxole.
One very easy way to make 1,3-benzodioxle is described here:
Obtain these 4 chemicals:
Catechol-110g
Dichloromethane(AR Grade)-100mL
Dimethylsulphoxide(AR Grade)-500mL
Sodium Hydroxide-83(AR Grade)g
The process is a dry reflux set up. Get a 2000mL reaction flask, a condenser and a drying tube packed with calcium chloride or other drying agent. The reaction must be stirred so have a clean stir bar ready (and set up the reflux on a stirring plate that you should own cause I told you to buy one in my grand post and I meant it. There is barely a single reaction you will do that doesn't involve heating or stirring or both.)
DMSO is a very common solvent that will come crystallised in the bottle. To melt place the bottle in a bowl of hot water for 30 minautes. If where you live is warm enough it may already be liquid. 500mL of this stuff goes straight into the reaction flask and start the stirrer. Next add the DCM, just pour it in. If you live in a humid environment (not here hehe) it may be a good idea to dry your two solvents with sodium sulphate. Also no matter where you live your glassware(metalware if you are ghetto) should be sterilized/dried by being baked at 425 degrees F (I assume the temperature is in F because you will bake it in a convential oven and none of them use Celcius. If you don't live in the US, convert it) for one hour. That should take care of any contaminants and moisture.
Use a DRY funnel and add the catechol slowly enough to not stop the stir bar, stopping the bar is bad. The solution will change colour to a dark green.
Add the sodium Hydroxide the same way as the catechol. Again this will slow down the stir bar so add slowly, you don't want it to stop your your yeilds will suffer. Now the reaction flask will warm up. Connect the condenser at this time and the drying tube. Make sure the drying agent is not clumped in a big lump wich can allow moisture to pass by, smash it all up with a pestle and mortar (a pestle and mortar is like a little bowl and a big stick with a rounded end shaped to fit the bowl. That way a substance can be placed in the bowl and pulverised by applying force with the stick. A mortar and pestle can be easily made out of something or another way of pulverizing the agent can be found by using your brain). It should completly cover the cotton woll in the drying tube. This is quite a reaction as it starts out and if the drying tube isn't firmly placed it will blow off and shoot across the kitchen so you should hold it in place for a few minautes or clamp it down to prevent this. It can also shoot off the plug if you are using a vacuum adaptor as your drying tube so tape or hold the plug. (If you don't know what the hell I'm talking about, read through my grand post, I tell you how to make your equiptment and perform the procedures there, or at least I think I do. I just skimmed it since I wrote it months ago and don't remember most of what I wrote and I kinda put all this information all over the place instead of together like it should be. I was really fucked up when I wrote that and I should rewrite some of it but that would be a big project. anywho, read from about the middle to 3/4 of the way down The section I marked off with "-----" going across the screen on the top and bottom is about the end of it as far as explaining how to make equiptment and perform chemistry. But I suggest reading the whole thing cause it's all a good read and you can make X by using my speed synthesis and starting with piperinol instead of benzaldehyde. Go on read it). With everything secured, start the heating gently. The reaction will already be going so things wont take long. After about 10 minautes the reaction will start in earnest, gasses will come out of the drying tube and the contents of the flask will be a n emerald green colour. This will last three to four minutes and then gradually slow down. This chemist talks about smelling the smelly DMSO so it sounds like you don't need to do this under a flowhood, but I still would to stay safe, this chemist could be half nuts by now from fumes. Once things die down take note of the time and leave it alone for half an hour. Then come back and remove the condenser, with the aid of a funnel add the water slowly, keep stirring. If the solution is too hot the water will evaporate and make a big mess. As the water is added you will notice that loads of stodgy crap will form. This is apperently normal. Just connect the condenser ready for distillation and connect a receiving flask of at least 500mL capacity. After about 30-45 minautes at about 85 degrees the distillate will start to come over. As it drops into the collection flask, a blob of oil will appear in the middle of the water. The oil appears clearer than the water, which will be milky in appearance. Now all there is to do is wait, adjust the heat so the temperature doesn't go above 100 degrees, this chemist suggests to have a cigerette, this is another no no in my opinion, even though I'm not a big bad chemist, but smoking and chemistry don't mix, go outside and smoke, I hope that's what he meant. He did say he was making it in the kitchen though so all this ghettoness is to be expected. After a couple hours you will notice that what's coming over contains less and less oil and eventually no oil, just water. At that point you stop the distillation, separate the oil from the water with a sepratory funnel, wash with water twice to remove any traces of milkiness. The product should be crystal clear, slightly more viscous than water, with a very strong odour. Credits for this Methylenation technique go to the chemist Merlin whose best yeild using it of benzodioxole from 110g catechol was 84g. See how well you can do. Merlin also mentions that this process will most likely have to be done twice to get enough benzodioxle for the next step towards making safrole or piperinol.
One more of the many methods of making 1,3-benzodioxle from pyrocatechol is probably the best if you can get the chemicals for it as it gives super high yeilds and takes place at room temperature. To a stirred suspension of 12.5g sodium hydride (NaH) in 200mL hexamethylphosphoric triamide (HMPT) is added a solution of 28.6g catechol in 100mL HMPT over a 10 minute period. A lot of bubbling will occur, and when it dies down 80g of DIM or 52g of DBM or 25.2g of DCM (the dichloromethane is probably easiest to get I think)is added and the solution stirred for 20 minutes. After the 20 minutes about 500mL cold dH2O is added and the whole thing extracted with ether. The solvent layer is dried through Na2SO4 and distilled to give 1,3-benzodioxole which will have the same characteristics noted in its description in the end of the above technique.
What is added to this document after its completion is based on the demand of the readers so if you want more techniques on how to make 1,3-benzodioxle or more techniques on how to do any of the other steps, let me know and I'll add them, I've got about 3 more ways to do this one alone. Volumes more then I am including on how to actually make safrole to an intermediate product then the intermediate product to X, so just ask and ye shall recieve.
For now I am just going to explain how to make safrole straight from 1,3-benzodioxole. You can also make 5-bromo-1,3-benzodioxole which can be made right into piperinol or safrole, but I'm gonna skip the bromination technique unless someone asks for it for now.
So this technique takes 34.3g of 1,3-benzodioxole, so you should have enough to run this process about two times with some left over from the first benzodioxole technique I went over. When you start out doing these you are in your experimentation stage and it is best to conduct these techniques exactly as written including amounts. Once you are experienced you can attempt to scale up or down your operation by MOLAR RATIO not weight ratio unless otherwise stated. Back to the topic at hand, in a very small flask add 7.2g of allyl chloride, your benzodioxole and 0.15g powdered Cu (which can be made by reducing a solution of CuSO4 with zinc dust). The solution is slowly heated to a mild boil for 10 hours with the temperature kept below 125 degrees C. Shake the mix with 5% NaOH solution, extract with ether and fractionally distill under a vacuum to get rid of unreacted 1,3benzodioxole and give you your safrole. Yeild is 30% that is pretty shitty, maybe I will add the bromo-benzodioxole techniques after all, but later for now I want to go on to the good stuff. First I gotta explain fractional distillation for this technique in case I didn't in my grand post.
Fractional distillation is basically distillation for substances with close boiling points, which makes distillation difficult especially since you have whacked out boiling points due to the altered pressure of the vacuum. So to solve this inbetween the condenser and the reaction flask you place another condenser. The difference is that this condenser has no water hoses attached to it as it is not going to be pumping water, instead its inner tube will be filled with beads to create more surface area. These beads should be glass or stainless steel as to not react with the chemicals they will be coming in contact with. On this website are pictures of fancy-pants professional labratory fractional distillation setup stuff:
http://orgchem.colorado.edu/hndbksupport/dist/distsetup/fractdist.html
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From this point on it is assumed that you have pure safrole in hand. If you can only get piperinol for some reason (it seems harder to get then safrole to me, but hey) and want to use these methods rather then giving my speed syntheses a try (I recomend my speed syntheses to make piperinol into X, but that's only cause I want feedback on whether or not my theory is true that it makes more potent X) reply or message me and I will add a section on making safrole out of piperinol. As far as I know there is no way to make piperinol out of safrole, but if you find one let me know and I'll throw it in here and give you credit if you want it. The following is the meat and potatoes of this thread, this is how you actually make X using the dreaded illegal precursor chemical safrole or isosafrole. There are many many ways to go about doing this and I will only add a few of my favorites but if you want more in a certain area request and I'll throw more in. Like I mentioned above, this document is being written by reader demand, I'll write first what I find most important, then anything more I add is what you want to read about. Especially reguarding the techniques/equiptment if I mention anything that I didn't explain fully either here or in the grand post then let me know so I can add it ASAP, if I don't know what I'm talking about I'll figure it out and put it in layman's terms for you guys, or chances are I already know what I'm talking about and just forgot to add it since I was spun out and thinking a mile a minaute when I wrote the grand post. But if I don't know what I'm talking about I know I can figure it out, I have with everything I know of so far that I've written about and I had to do some searching to find out how to do stuff like gel chromotography (which I actually didn't include since it's a pain in the ass) and precipitation, so I'll work hard for you guys.
Oh yes, the meat and potatoes, or since I'm a vegitarian the broccoli and cheese of this document. There are two big time main ways to make X and a few different side ways. I will go over two or three different techniques of each of the two big main ways and pick and choose a couple of promising other ways (the other ways tend to be more cutting edge so there is some risk and reward involved with trying them). We'll start with the two main ways which are what account for the very very vast most majority of all the X you see around. They are:
1)using a ketone intermediate: MDphenyl-2-propanone
2)using a beta-Nitropropene intermediate: MD-Phenyl-beta-Nitropropene
Both start out with safrole then make an extremely illegal intermediate chemical, then out of that intermediate chemical make an even more extremely illegal chemical known as MDMA. You can also make speed this way by starting out with Allylbenzene instead of safrole or even better I'm throwing in a direct benzene to P-2-P technique just for shits in giggles even though it is useless for making X since its catalyst destroys the MD ring of 1,3-benzodioxole. Using that if you are making speed the crappy, but extremely cheap and easy way, you don't even have to bother making allylbenzene, you can just start with benzene which is as cheap and common as dirt. Then making speed/X from the appropriate ketone is a peice of the cake, you'll see.
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We will start with making ketones out of safrole (for the rest of this document you speed makers who are too sissy to make speed the real way using ephedrine, which I outline in my grand post, just remember when I say safrole I mean allylbenzene, and after that just take the "MD" off the front of any chemical. Don't forget to account for the difference in atomic weight with the methylenedioxy ring gone which gives a difference of 44.01 amu. So you'll have to do mole problems using the molar ratios you calculate to figure how much weight of non methylenedioxy ringed substance to use in a reaction as opposed to how I am presenting it. If I havn't explained mole problems in the grand post then let me know and I'll write up an explanation and throw it in somewhere because they are pretty much the mathematical backbone of chemistry and knowing how to do them is crucial to doing chemistry, especially if you plan on scaling up or down an operation. They are so damn easy to do also, we're talking algebra I). Okay basically to make safrole into the ketone phenyl-2-propanone we must throw an oxygen atom onto the number 2 carbon of the propyl chain of safrole, and it must be double bonded. As I should have covered in my grand post, a ketone is when you have a carbon with a double bonded oxygen attached to it and anything attached to it and another anything attached to it as long as either of those anythings don't fufil the requirements to make it an acid, ester, or aldehyde instead. In this case it is a benzene ring and the number 1 carbon of the chain on one side and a methyl group (the number 3 carbon) on the other side, so it's a ketone. This is good as ketones have some special properties that will be covered later which make them easier to extract out of a solution. I've blabbed about this subject all I can, on to the techniques.
Okay, the by far best method for making safrole into MDP-2-P, and Strike agrees with me on this one so you know it's right, is the following one. The reason is simply because the chemicals required are so cheap and easy to get, and the yeild is good. Don't get me wrong the other method or methods I include after this one are better technically, they just use more expensive, less common chemicals. This one uses:
hydrogen peroxide
formic acid
sulfuric acid
and of course your safrole.
(oops I forgot:)
acetone
methanol
methanol is a common solvent. It is becoming less common because it is a deadly poison. You can still however find it as a solvent in some things like windshield wiper fluids and de-icers, antifreeze, glass cleaner, canned heat, paints, varnishes, paint thinners and removers. You'd have to seperate the methanol from all the other shit in any of those other products so your best bet is to just try and find a source to get it pure. As far as I know you should have no problem getting this from your local chemical supplier along with the rest of any solvents you are buying from them.
acetone is in nail polish remover. Just buy a big bottle of the highest concentration of acetone nail polish remover you can at the store. Hopefully you can get pure stuff, but I'm not a girl and I don't know much about nail polish remover so my guess is there is other shit in there. Look at the bottle, find out what it is, figure out if it will screw things up, and if it will, don't buy it. Especially since pure acetone should be found at one of those mega hardware stores. At such a store one can also find methanol (as mentioned above), DCM (as a constituent of some stripping agents), sodium hydroxide in the form of lye, and even sulfuric acid. Basically if you look at the chemical list above, I just rattled off most of it, a mega hardware store is your one stop shop for this synthesis, hit a grocery or drug store for the hydrogen peroxide, and if you have to make the formic acid, one of those hardware stores probably has the oxalic acid, if not a paint store of some kind should.
hydrogen peroxide was available in any grocery store last time I checked, sulfuric acid is used in like every other synthesis covered so you should be able to get this, if not message me and I'll find you a synthesis for sulfuric acid and put it in here somewhere, but you really should be able to buy it, you have to use so much of it all the time. Formic acid, you should be able to buy this stuff too, as it is used in commercial paint thinners. In case you can't buy it anywhere, here is how to make it out of two chemicals you can buy in any city easily, and in regular stores, not chemical supply stores. These two chemicals are glycerine and oxalic acid. Glycerine I'm almost sure you've heard of, is used in making soaps and cosmetic products (and I think explosives too, but I'm not sure on that one. Then again the point of our chemistry here is to NOT blow up so don't even think about it.) If you shop around you should be able to find it in a store, if not go to a chemical supplier and if they ask you about it say you are making soaps. They probably wont belive you if you are buying it with a bunch of solvents like DMSO, or reagents like your oxalic acid, so I'd have a few different chemical suppliers that I go to if I were you and like buy all of my reagents one place, all my solvents one place, etc. Unless you find that one supplier is really cool/groovy and doesn't give a flying fuck what you do with the chemicals. Many are like that you'd be surprised. Oxalic acid, though you probably havn't heard of it, should be even easier to get then the glycerine. Oxalic acid is used to refinish wood furnature. Try and find a store that sells chemicals you'd use to bleach wood furnature, OR try using a little google. Using google I found a source for oxalic acid charging $12 for 1 lb or $20 for 2 lb of pure oxalic acid, no joke. Unfortunatly for you I cannot list it here due to forum rules, but if you use google, you'll find it. Or even better then trusting some shady internet site is finding a store that sells it, I wouldn't be surprised if Home Depot or someplace like that carried it. Now with glycerine and oxalic acid in hand you are ready to make formic acid:
Mix an equal amount of glycerine and oxalic acid and place in a flask. Heat this mixture at 75-90°C. Continue heating until no more CO2 bubbles out. Fresh oxalic acid is added and the process continued. When enough acid is made, distill it over using the proper apparatus and raising the temperature with an oil bath. 90% formic acid is collected. Alternatively, you can place the mixture in a distillation apparatus with a vacuum connection. Read the temperature with the thermometer placed into the mixture. Heat the mixture to ~90°C, but while under reduced pressure. As the reaction proceeds the formic acid will distill over. This takes about 4 to 5 hours for 500g of glycerine and 500g of oxalic acid.
To make things way easier and take tons less time, you'll also want sodium bisulfite, I will explain when the time is right. Instead of sodium bisulfite you can use sodium metabisulfite and it works just as well, many companies don't carry sodium bisulfite.
A large flask or glass tea jug is placed in a tray of ice on top of a magnetic stir plate. Into th eflask is poured 340g of 30% hydrogen peroxide. Always store your hydrogen peroxide in a fridge or it will degrade over time. Also pour in 1500g of 88% formic acid. There will be heavy fumes when the formic acid is being dumped into the reaction flask, but after the initial disturbance, the fumes will die down. Formic acid is considered a dangerous chemical so a hood is still a good idea. It's always a good idea, cause you never know when a synthesis technique completly forgets about some deadly fumes that a reaction emits. 324g isosafrole (it says isosafrole here, then the diagram above in the book shows a picture of safrole, what gives? oh well, try it with either or see what works, get back to me. If only isosafrole works in this reaction, there is an easy way to make it from safrole that I can include in the document) and 1000mL acetone are mixed in a PP container then poured into a separatory funnel. The separatory funnel is placed so that the nosel is ready to drip down into the reaction flask. The acetone solution is added drop by drop into the cold formic solution so that the temperature stays between 10-20 degrees C. Keep the ice bath well stocked and the dripping under control and make sure it stays below 20. The solution will start off clear to pale yellow, then will turn orangy as dripping continues. After about 200mLs of addition the temperature shouldn't rise so much if the dripping is increased. When addition is complete, the thermometer and seperatory funnel are removed and a peice of foil is placed on the top of the reaction flask. The reaction flask is left stirring overnight and no more ice is added to the ice bath, so as the ice melts, the reaction slowly comes to room temperature.
The next day it is time to get rid of all the leftover formic acid then do the reflux with sulfuric acid to end up with the ketone. The first step is getting out the leftover acetone. This is done by taking the reaction flask from the last step and just hooking it right up as the flask for boiling in a vacuum distillation setup. The acetone will come over first, then done. The second step is getting rid of that formic acid. You can do this through tedious distillation, but I don't recommend it, instead you can do an extraction in the following manner:
netralize the formic acid mix with 25% NaOH, the layers seperate out nicely. It takes a lot of NaOH to neutralize the solution so you'll need a big sepratory funnel, or you'll have to do it in batches at a time in your smaller one. You'll need ph testing equiptment, a digital ph meter is a little pricey but well worth the money. Keep testing the formic acid mix as you add the NaOH and afteryou hit ph 4.5 add it very carefully, cause it will start to climb up to 9+ real quick. You can then back extract the water with DCM or better yet ether because ifyou use too much DCM when extracting it sinks to the bottom and some product floats on top, giving you three layers.
If you can't do the above extraction, just keep the distillation setup as is from distilling out the acetone and keep distilling until all the formic acid comes over. This will take a while.
No matter how you got to this point, you should have a black syrup in the bottom of your flask. Into it pour 500mL methanol and 2500mL 15% sulfuric acid solution. If you don't have a big enough flask, you'll have to half or third the syrup stuff and do it in batches. After adding the methanol and sulfuric acid the heavy black layer will form beads and sink to the bottom and the solution itself will get kind of milky and hazy. Now you slap the condenser and dryinig tube on top of the reaction flask and reflux for three hours. After that, let it cool down to room temperature. Then, since all the oil will be sitting at the bottom of the flask, you decant as much of the water as possible, add fresh water, stir, decant again. Do this three times to remove any traces of sulfuric acid left in the oil. Now we want to get our MDP-2-P out of the oil. This is where the sodium bisulfite comes in. Dissolve as much sodium bisulfite as will dissolve in a given amount of water. This makes a saturated solution. Now add the oil to this solution and stir for 30 minutes. The temperature of the reaction will rise and a big mass of crystals will form. These crystals which will look a lot like chicken fat are your MDP2P. Let the solution cool then seperate the crystals from the solution by vacuum filtration. Wash with a little clean dH2O, then wash with a couple hundred mL of ether, DCM, or benzene. Scrape the crystals into a flask and then add 300mL of 10%HCl solution. Stir for another 30 minutes. The MDP2P is taken up with ether, dried and removed of the solvent to give pure MD-P2P.
That method uses really easy to get chemicals but is quite tedious. I will add the most popular method of making MD-P2P, named the wacker oxidation method later, actually it will be a variation of the commonly used wacker oxidation method that blows the original one that everyone is still using on the streets, away. For now I feel like getting into how to make X out of that MD-P2P, it's really easy, you'll shit your pants when you read this next section.
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Making X out of MD-P2P is much easier then making MD-P2P from safrole. The following method is the most common street method for making X, and there is a reason for it. If you have read up on any street drug chemistry or hung out with Outlaw Motorcycle Gang members you may already be familiar with this method, as it is the same method they use to make crank.
It is so great because it uses ordinary household foil. The yeild is a little low at 50-60%, but hey you are reacting your MD-P2P with aluminum foil you can buy at the grocery store, what do you expect. It doesn't exactly use JUST aluminum foil as is, it uses amalgamated aluminum which is easy to make out of aluminum foil, by reacting it with mercuric chloride. Getting the mercuric chloride may proove to be a bitch as it is a very dangerous chemical but you don't need hardly any of it, so your small order of it should slip by unquestioned when you are buying chemicals. If you happen to not be able to buy it, there are a couple ways to make it. One is to obtain mercury which should be pretty easy and obtain some chlorine gas and react the two. The other way is to try and get ahold of some mercuric sulfate and sublime a mixture of it and common salt. mercuric sulfate also seems like it would be a bitch to get, but looking at the MSDSes doesn't appear to be quite as dangerous as the mercuric chloride, but maybe it is the same or more dangerous, I only skimmed the sheets, so I dunno. I'd try buying it straight up first since you don't need that much, then I'd try getting some mercury and chlorine gas since you should be able to get both of those. I don't know exactly how to do this reaction though, looks like I'll be hitting the library, but as I said before from what I've read getting some mercuric chloride should be no problem.
Now this technique with just the amalgamated aluminum makes MDA, this is X but without the methyl group on the nitrogen atom. Lets delve into what exactly the extra methyl group does for you, and you can decide for yourself whether or not its worth the trouble of throwing it on there. MDA and amphetamine are the easiest to make, involve the least watched chemicals, and are the strongest. MDMA and speed although less strong and shorter lasting, are perceived by many as "better" because the highs they produce are smoother and more pleasant. This is not necessarily true as the degrees of differences between MDA and MDMA or amphetamine and speed are very subjective. Strike goes on to strongly recommend making MDA, and talks about why it is better. Basically the more carbon atoms you slam on the nitrogen atom, the weaker the drug becomes. There is actually MDethylamphetamine which is two carbons attached to the nitrogen atom, and it is weaker then MDMA, but still retains some activity. Basically the easy way is to stick with MDA and you will get a stronger longer lasting drug out of it, it just may not be quite as smooth as the MDMA you are used to, on the other hand you wont have to use methylamine to make it, and methylamine is an extremely watched chemical that can get you in big big trouble.
Unfortunatly the method of making MDA with AlHg sucks ass, but a brilliant chemist named Ritter came up with a new method of making MDMA without th insidious methylamine. This is what I will share with you. It uses nitromethane instead of methylamine. So now our reacting chemicals shall be:
MD-P2P
AlHg
Nitromethane(MeNO2)
Where do you find Nitromethane, easy just go down to your local drag strip or auto parts store and pick up a gallon or two for doping your high performance car's fuel. It's also available up to 40% pure in RC model fuels. If you are using the RC model fuel you will have to fractionally distill the nitromethane out of the mixture, it has a bp of 101 degrees C.
Set up a 2 liter two or three-neck flask with an addition funnel and a reflux condenser and provide with a heat source. Not much heat is needed here so a water bath might help keep the temperature down. Stuff 55 grams of one-inch squares of aluminum foil into the flask. Now something that must be mentioned is that you do NOT want to use the thin crappy food grade aluminum foil, that will react too fast and could cause an explosion. You want that thick aluminum foil you use to smoke heroin off of, you know what I'm talking about. The best foil is available in 4"x4" sheets 0.04mm thick, neatly separated from each other with a sheet of tissue paper. This foil is used for sealing flasks. If you don't have access to this wonderful foil, then just use the heroin smoking heavy-duty foil, just not the food grade cheap stuff. Remember to keep a close eye on the reaction rate.
Anywho, fill the seperatory funnel with 50 grams of MDP2P and 50grams or 39mL nitromethane dissolved in 200mL methanol. In another 1 liter vessel add 1.5g HgCl2 to a liter of methanol and allow all solids to dissolve. Very carefully, as I mentioned before HgCl2 is deadly poisonous, use your hood, gas mask, biosuit, everything to protect yo ass, pour the methanolic solution of HgCl2 onto the aluminum foil pieces in the flask and stand back and watch the magic begin. After about 5-10 minutes the bubbling should be sufficient and you may start adding the methanolic mixture of nitromethane and MDP2P drop by drop from the seperatory funnel. As time progresses, the reaction may heat up to the point of boiling and refluxing of the alcohol will occur. This is no problem as the 65 degree C boiling point of methanol is perfect for this reaction. The addition should take roughly one hour and the mixture should be allowed to react for at least 4-6 hours after or until all pieces of aluminum are reacted into a gray suspension. Temperature control needs to be addressed here. If the reaction proceeds under ideal conditions, it will run exactly as described above. If not, and more commonly, the reaction will start to slow down halfway through requiring external heating to maintain a good reaction rate. If things are going badly (no not assuming you blew up, that's if things are going really really badly), an addition of another gram of HgCl2 in methanol solution added to the mix will kick it back in. The next step is the easy part but it must be done right as you want your final product to have NO mercury contamination. Mercury is bad and that's why the HgCl2 may be a bitch to find. Well mercury can be good, hell it can be great, but it's bad for you, and that's why you want to get rid of it in this step. Mix about 1.5 or 2 liters of 35% NaOH soluton and allow to cool. Slowly add the gray aluminum gook produced in the first reaction to the NaOH solution and pour into a large seperatory funnel. Two distinct layers will appear after sitting for maybe an hour, the top being a reddish alcoholic solution of product and the bottom garbage NaOH/Al(OH)3. Simply separate off the garbage bottom layer and discard. Don't worry there's no product tied up in it, and remember that no filtration is needed anywhere in this recovery process compared to other synths out there. Take the top layer and evaporate off the methanol to give an amazing yield of impure amine and a little bit of water. But we are not done yet, there is still the mercury salts in the mix. We must get rid of them, or you are a bad cook. You can poision your customers all you want, but I'm gonna tell you how to do this right, so don't blame me if you skip this last important step. Dissolve the crude product in about a liter of toluene (toluene is watched so be careful, a hardware store may sell it even though it is watched so look around. If you can't find it, as you probably can't, the DEA hates toluene, you can make it out of Benzene by reacting the benzene with CH3Cl in the presence of AlCl3. I'll have to look more in depth for further info on this reaction. I'm not finding shit on the net about it besides what I've told you so I'll have to hit a sci journal. I'll probably be posting a better technique using a higher powered catalyst later anyways so you may not even need to worry about finding the HgCl2 or toluene. For now what you see is what you get). Allow me to finish, The crude product has been dissolved in toluene, now wash the product/toluene with several portions of water in a seperatory funnel and finally with saturated NaCl solution. Dry the toluene with about 50g anhydrous MgSO4. You make the anhydrous MgSO4 by heating drug store epsom salts in the oven at 400 degrees F for an hour, cooling, then powdering. After sitting for an hour or until the toluene is no longer cloudy, chill the dried toluene solution of freebase in the freezer and bubble away with HCl gas to yeild pure MDMA crystals. If they are a little discolored they can be easily cleaned up with an acetone rinse.
There is one more very promising, but very new P2P->amphetamine technique I am going to share with you all, but I will add that later. For now I have completly outlined one of the many ways you can fully synthesize X. Remember don't be afraid to ask questions about anything I covered, I wrote this for YOU.
There are many many ways to make X, the most popular are either via the ketone MDP-2-P or B-Nitropropenes. The most important part is obtaining a precursor chemical, which can be one of three chemicals, all are heavily watched so you have to be crafty to get ahold of them. The three chemicals are Safrole, Isosafrole, and Piperinol. I will start out with some ways to obtain them.
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The easiest way to obtain a precursor chemical is to find some kind of oil or substance already containing a percentage of the chemical in it already and isolating it.
The most common way of getting safrole is via sassafras oil. There are two kinds of this, the American kind and the Brazillian kind. The American kind contains about 80% safrole and the Brazillian about 90-95% (the Brazillian kind can obviously be used as is with no further purification, since it is already almost pure safrole). This oil can be obtained from health food stores or through fragrance or perfume supply companies. Be very careful when purchasing as it is well known what this is used for; it is best to have someone who isn't you buy it for you, especially in any kind of quantity. Other oils containing safrole in about the 40-50% are camphor oil, artificial sassafras oil, and betel leaf oil. Smaller amounts can be found in the oils of cinnamon, mace, and nutmeg. If you live in the eastern US along the eastern seaboard or the Appalachian mountain regions you can actually find the sassafras tree and the trunk and root bark of older, mature trees can be steam distilled to produce safrole. Safrole's boiling point is 234 degrees C at 1atm so get distillin'.
Or you could really luck out and be from Georgia or Florida and have a great plant called the yellow anisetree grow natively in thier area. This tree is a shrub that grows in the low woods and swamps throughout the coastal plains from Florida to Georgia. The oil from its leaves is more than 90% safrole and can be used as is once extracted from the leaves of a plant.
Isosafrole does not occur in nature and can only be manufactured from safrole. It is pretty much interchangeable with safrole as a precursor chemical so we will skip it.
One good idea, even when dealing with the almost pure safrole oils that was forgotten is that you should try and get rid of any eugenol contaminating the oil, as it reacts similar to safrole. To do this simply put the oil in a PP container and stir with an equal amount of 3-5% sodium hydroxide solution. Little white crystals of eugenol anion will form in the water layer. The water layer is poured off and saved (Eugenol can be useful). Wash the oil 3 times while being stirred, then place in a cooking pot and boil at 100 degrees C for a few minutes to boil off all the water.
I dun remember what has piperinol in it except pepper. But it is a bitch to isolate from the pepper and yeilds are low apperently so just try and go for safrole, since to use this guide you will have to make piperinol into safrole anyways. If you do end up with piperinol somehow, try substituting it for benzaldehyde in my speed making technique in the "grand post for all D&B" it should work and could possibly make more potent X theoretically. Of course I've never done any of this shit IRL, I've just read a lot up on it all so I'm interested in knowing how it works, message me if you ever try it. :shifty:
If you were able to use any of the above methods to obtain pure or mostly pure safrole, isosafrole, or piperinol, you can skip to section 3. Otherwise you gotta wade through section two directly below. Don't worry if I were to ever make X I'd have to make my precursors too since I'm too paranoid to go out and buy sassafras oil and I don't live anywhere near sassafras trees or Yellow Anisetrees, the closest wild one of either to me is probably 2000 miles away or so. I also wont go to a nursery and buy a tree to mutalate to make X cause I kind of have a thing against mutalating my own plants, even for drugs. Even though as you all know I have no problem ripping off wild cactus or cactus belonging to other people in thier yards for drugs :D
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At last, if you can't get precursors any of the ways above, you gotta make them from scratch and this is a bitch, and dangerous(actually I think I left the dangerous process out for now, but I'm gonna add it later methinks, so beee careful). It is recommended you have some labrotory experience before ever attempting any of this because, yeah some steps are dangerous.
Basically you start with pyrocatechol, this chemical is common and not watched and should be no problem to get. If it is a problem to get and you can get Salicyladehyde or Guaiacol instead, you can make pyrocatechol out of it, but I don't want to waste my time explaining this if I don't have to, so if this happens to be your case message me or reply stating the situation and I will add this process, otherwise I'll just assume you can get the catechol.
pyrocatechol is a benzene ring with alcohol molecules on two adjacent carbons. The goal of this process is to connect them into a methylenedioxy ring and form 1,3-benzodioxole.
One very easy way to make 1,3-benzodioxle is described here:
Obtain these 4 chemicals:
Catechol-110g
Dichloromethane(AR Grade)-100mL
Dimethylsulphoxide(AR Grade)-500mL
Sodium Hydroxide-83(AR Grade)g
The process is a dry reflux set up. Get a 2000mL reaction flask, a condenser and a drying tube packed with calcium chloride or other drying agent. The reaction must be stirred so have a clean stir bar ready (and set up the reflux on a stirring plate that you should own cause I told you to buy one in my grand post and I meant it. There is barely a single reaction you will do that doesn't involve heating or stirring or both.)
DMSO is a very common solvent that will come crystallised in the bottle. To melt place the bottle in a bowl of hot water for 30 minautes. If where you live is warm enough it may already be liquid. 500mL of this stuff goes straight into the reaction flask and start the stirrer. Next add the DCM, just pour it in. If you live in a humid environment (not here hehe) it may be a good idea to dry your two solvents with sodium sulphate. Also no matter where you live your glassware(metalware if you are ghetto) should be sterilized/dried by being baked at 425 degrees F (I assume the temperature is in F because you will bake it in a convential oven and none of them use Celcius. If you don't live in the US, convert it) for one hour. That should take care of any contaminants and moisture.
Use a DRY funnel and add the catechol slowly enough to not stop the stir bar, stopping the bar is bad. The solution will change colour to a dark green.
Add the sodium Hydroxide the same way as the catechol. Again this will slow down the stir bar so add slowly, you don't want it to stop your your yeilds will suffer. Now the reaction flask will warm up. Connect the condenser at this time and the drying tube. Make sure the drying agent is not clumped in a big lump wich can allow moisture to pass by, smash it all up with a pestle and mortar (a pestle and mortar is like a little bowl and a big stick with a rounded end shaped to fit the bowl. That way a substance can be placed in the bowl and pulverised by applying force with the stick. A mortar and pestle can be easily made out of something or another way of pulverizing the agent can be found by using your brain). It should completly cover the cotton woll in the drying tube. This is quite a reaction as it starts out and if the drying tube isn't firmly placed it will blow off and shoot across the kitchen so you should hold it in place for a few minautes or clamp it down to prevent this. It can also shoot off the plug if you are using a vacuum adaptor as your drying tube so tape or hold the plug. (If you don't know what the hell I'm talking about, read through my grand post, I tell you how to make your equiptment and perform the procedures there, or at least I think I do. I just skimmed it since I wrote it months ago and don't remember most of what I wrote and I kinda put all this information all over the place instead of together like it should be. I was really fucked up when I wrote that and I should rewrite some of it but that would be a big project. anywho, read from about the middle to 3/4 of the way down The section I marked off with "-----" going across the screen on the top and bottom is about the end of it as far as explaining how to make equiptment and perform chemistry. But I suggest reading the whole thing cause it's all a good read and you can make X by using my speed synthesis and starting with piperinol instead of benzaldehyde. Go on read it). With everything secured, start the heating gently. The reaction will already be going so things wont take long. After about 10 minautes the reaction will start in earnest, gasses will come out of the drying tube and the contents of the flask will be a n emerald green colour. This will last three to four minutes and then gradually slow down. This chemist talks about smelling the smelly DMSO so it sounds like you don't need to do this under a flowhood, but I still would to stay safe, this chemist could be half nuts by now from fumes. Once things die down take note of the time and leave it alone for half an hour. Then come back and remove the condenser, with the aid of a funnel add the water slowly, keep stirring. If the solution is too hot the water will evaporate and make a big mess. As the water is added you will notice that loads of stodgy crap will form. This is apperently normal. Just connect the condenser ready for distillation and connect a receiving flask of at least 500mL capacity. After about 30-45 minautes at about 85 degrees the distillate will start to come over. As it drops into the collection flask, a blob of oil will appear in the middle of the water. The oil appears clearer than the water, which will be milky in appearance. Now all there is to do is wait, adjust the heat so the temperature doesn't go above 100 degrees, this chemist suggests to have a cigerette, this is another no no in my opinion, even though I'm not a big bad chemist, but smoking and chemistry don't mix, go outside and smoke, I hope that's what he meant. He did say he was making it in the kitchen though so all this ghettoness is to be expected. After a couple hours you will notice that what's coming over contains less and less oil and eventually no oil, just water. At that point you stop the distillation, separate the oil from the water with a sepratory funnel, wash with water twice to remove any traces of milkiness. The product should be crystal clear, slightly more viscous than water, with a very strong odour. Credits for this Methylenation technique go to the chemist Merlin whose best yeild using it of benzodioxole from 110g catechol was 84g. See how well you can do. Merlin also mentions that this process will most likely have to be done twice to get enough benzodioxle for the next step towards making safrole or piperinol.
One more of the many methods of making 1,3-benzodioxle from pyrocatechol is probably the best if you can get the chemicals for it as it gives super high yeilds and takes place at room temperature. To a stirred suspension of 12.5g sodium hydride (NaH) in 200mL hexamethylphosphoric triamide (HMPT) is added a solution of 28.6g catechol in 100mL HMPT over a 10 minute period. A lot of bubbling will occur, and when it dies down 80g of DIM or 52g of DBM or 25.2g of DCM (the dichloromethane is probably easiest to get I think)is added and the solution stirred for 20 minutes. After the 20 minutes about 500mL cold dH2O is added and the whole thing extracted with ether. The solvent layer is dried through Na2SO4 and distilled to give 1,3-benzodioxole which will have the same characteristics noted in its description in the end of the above technique.
What is added to this document after its completion is based on the demand of the readers so if you want more techniques on how to make 1,3-benzodioxle or more techniques on how to do any of the other steps, let me know and I'll add them, I've got about 3 more ways to do this one alone. Volumes more then I am including on how to actually make safrole to an intermediate product then the intermediate product to X, so just ask and ye shall recieve.
For now I am just going to explain how to make safrole straight from 1,3-benzodioxole. You can also make 5-bromo-1,3-benzodioxole which can be made right into piperinol or safrole, but I'm gonna skip the bromination technique unless someone asks for it for now.
So this technique takes 34.3g of 1,3-benzodioxole, so you should have enough to run this process about two times with some left over from the first benzodioxole technique I went over. When you start out doing these you are in your experimentation stage and it is best to conduct these techniques exactly as written including amounts. Once you are experienced you can attempt to scale up or down your operation by MOLAR RATIO not weight ratio unless otherwise stated. Back to the topic at hand, in a very small flask add 7.2g of allyl chloride, your benzodioxole and 0.15g powdered Cu (which can be made by reducing a solution of CuSO4 with zinc dust). The solution is slowly heated to a mild boil for 10 hours with the temperature kept below 125 degrees C. Shake the mix with 5% NaOH solution, extract with ether and fractionally distill under a vacuum to get rid of unreacted 1,3benzodioxole and give you your safrole. Yeild is 30% that is pretty shitty, maybe I will add the bromo-benzodioxole techniques after all, but later for now I want to go on to the good stuff. First I gotta explain fractional distillation for this technique in case I didn't in my grand post.
Fractional distillation is basically distillation for substances with close boiling points, which makes distillation difficult especially since you have whacked out boiling points due to the altered pressure of the vacuum. So to solve this inbetween the condenser and the reaction flask you place another condenser. The difference is that this condenser has no water hoses attached to it as it is not going to be pumping water, instead its inner tube will be filled with beads to create more surface area. These beads should be glass or stainless steel as to not react with the chemicals they will be coming in contact with. On this website are pictures of fancy-pants professional labratory fractional distillation setup stuff:
http://orgchem.colorado.edu/hndbksupport/dist/distsetup/fractdist.html
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From this point on it is assumed that you have pure safrole in hand. If you can only get piperinol for some reason (it seems harder to get then safrole to me, but hey) and want to use these methods rather then giving my speed syntheses a try (I recomend my speed syntheses to make piperinol into X, but that's only cause I want feedback on whether or not my theory is true that it makes more potent X) reply or message me and I will add a section on making safrole out of piperinol. As far as I know there is no way to make piperinol out of safrole, but if you find one let me know and I'll throw it in here and give you credit if you want it. The following is the meat and potatoes of this thread, this is how you actually make X using the dreaded illegal precursor chemical safrole or isosafrole. There are many many ways to go about doing this and I will only add a few of my favorites but if you want more in a certain area request and I'll throw more in. Like I mentioned above, this document is being written by reader demand, I'll write first what I find most important, then anything more I add is what you want to read about. Especially reguarding the techniques/equiptment if I mention anything that I didn't explain fully either here or in the grand post then let me know so I can add it ASAP, if I don't know what I'm talking about I'll figure it out and put it in layman's terms for you guys, or chances are I already know what I'm talking about and just forgot to add it since I was spun out and thinking a mile a minaute when I wrote the grand post. But if I don't know what I'm talking about I know I can figure it out, I have with everything I know of so far that I've written about and I had to do some searching to find out how to do stuff like gel chromotography (which I actually didn't include since it's a pain in the ass) and precipitation, so I'll work hard for you guys.
Oh yes, the meat and potatoes, or since I'm a vegitarian the broccoli and cheese of this document. There are two big time main ways to make X and a few different side ways. I will go over two or three different techniques of each of the two big main ways and pick and choose a couple of promising other ways (the other ways tend to be more cutting edge so there is some risk and reward involved with trying them). We'll start with the two main ways which are what account for the very very vast most majority of all the X you see around. They are:
1)using a ketone intermediate: MDphenyl-2-propanone
2)using a beta-Nitropropene intermediate: MD-Phenyl-beta-Nitropropene
Both start out with safrole then make an extremely illegal intermediate chemical, then out of that intermediate chemical make an even more extremely illegal chemical known as MDMA. You can also make speed this way by starting out with Allylbenzene instead of safrole or even better I'm throwing in a direct benzene to P-2-P technique just for shits in giggles even though it is useless for making X since its catalyst destroys the MD ring of 1,3-benzodioxole. Using that if you are making speed the crappy, but extremely cheap and easy way, you don't even have to bother making allylbenzene, you can just start with benzene which is as cheap and common as dirt. Then making speed/X from the appropriate ketone is a peice of the cake, you'll see.
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We will start with making ketones out of safrole (for the rest of this document you speed makers who are too sissy to make speed the real way using ephedrine, which I outline in my grand post, just remember when I say safrole I mean allylbenzene, and after that just take the "MD" off the front of any chemical. Don't forget to account for the difference in atomic weight with the methylenedioxy ring gone which gives a difference of 44.01 amu. So you'll have to do mole problems using the molar ratios you calculate to figure how much weight of non methylenedioxy ringed substance to use in a reaction as opposed to how I am presenting it. If I havn't explained mole problems in the grand post then let me know and I'll write up an explanation and throw it in somewhere because they are pretty much the mathematical backbone of chemistry and knowing how to do them is crucial to doing chemistry, especially if you plan on scaling up or down an operation. They are so damn easy to do also, we're talking algebra I). Okay basically to make safrole into the ketone phenyl-2-propanone we must throw an oxygen atom onto the number 2 carbon of the propyl chain of safrole, and it must be double bonded. As I should have covered in my grand post, a ketone is when you have a carbon with a double bonded oxygen attached to it and anything attached to it and another anything attached to it as long as either of those anythings don't fufil the requirements to make it an acid, ester, or aldehyde instead. In this case it is a benzene ring and the number 1 carbon of the chain on one side and a methyl group (the number 3 carbon) on the other side, so it's a ketone. This is good as ketones have some special properties that will be covered later which make them easier to extract out of a solution. I've blabbed about this subject all I can, on to the techniques.
Okay, the by far best method for making safrole into MDP-2-P, and Strike agrees with me on this one so you know it's right, is the following one. The reason is simply because the chemicals required are so cheap and easy to get, and the yeild is good. Don't get me wrong the other method or methods I include after this one are better technically, they just use more expensive, less common chemicals. This one uses:
hydrogen peroxide
formic acid
sulfuric acid
and of course your safrole.
(oops I forgot:)
acetone
methanol
methanol is a common solvent. It is becoming less common because it is a deadly poison. You can still however find it as a solvent in some things like windshield wiper fluids and de-icers, antifreeze, glass cleaner, canned heat, paints, varnishes, paint thinners and removers. You'd have to seperate the methanol from all the other shit in any of those other products so your best bet is to just try and find a source to get it pure. As far as I know you should have no problem getting this from your local chemical supplier along with the rest of any solvents you are buying from them.
acetone is in nail polish remover. Just buy a big bottle of the highest concentration of acetone nail polish remover you can at the store. Hopefully you can get pure stuff, but I'm not a girl and I don't know much about nail polish remover so my guess is there is other shit in there. Look at the bottle, find out what it is, figure out if it will screw things up, and if it will, don't buy it. Especially since pure acetone should be found at one of those mega hardware stores. At such a store one can also find methanol (as mentioned above), DCM (as a constituent of some stripping agents), sodium hydroxide in the form of lye, and even sulfuric acid. Basically if you look at the chemical list above, I just rattled off most of it, a mega hardware store is your one stop shop for this synthesis, hit a grocery or drug store for the hydrogen peroxide, and if you have to make the formic acid, one of those hardware stores probably has the oxalic acid, if not a paint store of some kind should.
hydrogen peroxide was available in any grocery store last time I checked, sulfuric acid is used in like every other synthesis covered so you should be able to get this, if not message me and I'll find you a synthesis for sulfuric acid and put it in here somewhere, but you really should be able to buy it, you have to use so much of it all the time. Formic acid, you should be able to buy this stuff too, as it is used in commercial paint thinners. In case you can't buy it anywhere, here is how to make it out of two chemicals you can buy in any city easily, and in regular stores, not chemical supply stores. These two chemicals are glycerine and oxalic acid. Glycerine I'm almost sure you've heard of, is used in making soaps and cosmetic products (and I think explosives too, but I'm not sure on that one. Then again the point of our chemistry here is to NOT blow up so don't even think about it.) If you shop around you should be able to find it in a store, if not go to a chemical supplier and if they ask you about it say you are making soaps. They probably wont belive you if you are buying it with a bunch of solvents like DMSO, or reagents like your oxalic acid, so I'd have a few different chemical suppliers that I go to if I were you and like buy all of my reagents one place, all my solvents one place, etc. Unless you find that one supplier is really cool/groovy and doesn't give a flying fuck what you do with the chemicals. Many are like that you'd be surprised. Oxalic acid, though you probably havn't heard of it, should be even easier to get then the glycerine. Oxalic acid is used to refinish wood furnature. Try and find a store that sells chemicals you'd use to bleach wood furnature, OR try using a little google. Using google I found a source for oxalic acid charging $12 for 1 lb or $20 for 2 lb of pure oxalic acid, no joke. Unfortunatly for you I cannot list it here due to forum rules, but if you use google, you'll find it. Or even better then trusting some shady internet site is finding a store that sells it, I wouldn't be surprised if Home Depot or someplace like that carried it. Now with glycerine and oxalic acid in hand you are ready to make formic acid:
Mix an equal amount of glycerine and oxalic acid and place in a flask. Heat this mixture at 75-90°C. Continue heating until no more CO2 bubbles out. Fresh oxalic acid is added and the process continued. When enough acid is made, distill it over using the proper apparatus and raising the temperature with an oil bath. 90% formic acid is collected. Alternatively, you can place the mixture in a distillation apparatus with a vacuum connection. Read the temperature with the thermometer placed into the mixture. Heat the mixture to ~90°C, but while under reduced pressure. As the reaction proceeds the formic acid will distill over. This takes about 4 to 5 hours for 500g of glycerine and 500g of oxalic acid.
To make things way easier and take tons less time, you'll also want sodium bisulfite, I will explain when the time is right. Instead of sodium bisulfite you can use sodium metabisulfite and it works just as well, many companies don't carry sodium bisulfite.
A large flask or glass tea jug is placed in a tray of ice on top of a magnetic stir plate. Into th eflask is poured 340g of 30% hydrogen peroxide. Always store your hydrogen peroxide in a fridge or it will degrade over time. Also pour in 1500g of 88% formic acid. There will be heavy fumes when the formic acid is being dumped into the reaction flask, but after the initial disturbance, the fumes will die down. Formic acid is considered a dangerous chemical so a hood is still a good idea. It's always a good idea, cause you never know when a synthesis technique completly forgets about some deadly fumes that a reaction emits. 324g isosafrole (it says isosafrole here, then the diagram above in the book shows a picture of safrole, what gives? oh well, try it with either or see what works, get back to me. If only isosafrole works in this reaction, there is an easy way to make it from safrole that I can include in the document) and 1000mL acetone are mixed in a PP container then poured into a separatory funnel. The separatory funnel is placed so that the nosel is ready to drip down into the reaction flask. The acetone solution is added drop by drop into the cold formic solution so that the temperature stays between 10-20 degrees C. Keep the ice bath well stocked and the dripping under control and make sure it stays below 20. The solution will start off clear to pale yellow, then will turn orangy as dripping continues. After about 200mLs of addition the temperature shouldn't rise so much if the dripping is increased. When addition is complete, the thermometer and seperatory funnel are removed and a peice of foil is placed on the top of the reaction flask. The reaction flask is left stirring overnight and no more ice is added to the ice bath, so as the ice melts, the reaction slowly comes to room temperature.
The next day it is time to get rid of all the leftover formic acid then do the reflux with sulfuric acid to end up with the ketone. The first step is getting out the leftover acetone. This is done by taking the reaction flask from the last step and just hooking it right up as the flask for boiling in a vacuum distillation setup. The acetone will come over first, then done. The second step is getting rid of that formic acid. You can do this through tedious distillation, but I don't recommend it, instead you can do an extraction in the following manner:
netralize the formic acid mix with 25% NaOH, the layers seperate out nicely. It takes a lot of NaOH to neutralize the solution so you'll need a big sepratory funnel, or you'll have to do it in batches at a time in your smaller one. You'll need ph testing equiptment, a digital ph meter is a little pricey but well worth the money. Keep testing the formic acid mix as you add the NaOH and afteryou hit ph 4.5 add it very carefully, cause it will start to climb up to 9+ real quick. You can then back extract the water with DCM or better yet ether because ifyou use too much DCM when extracting it sinks to the bottom and some product floats on top, giving you three layers.
If you can't do the above extraction, just keep the distillation setup as is from distilling out the acetone and keep distilling until all the formic acid comes over. This will take a while.
No matter how you got to this point, you should have a black syrup in the bottom of your flask. Into it pour 500mL methanol and 2500mL 15% sulfuric acid solution. If you don't have a big enough flask, you'll have to half or third the syrup stuff and do it in batches. After adding the methanol and sulfuric acid the heavy black layer will form beads and sink to the bottom and the solution itself will get kind of milky and hazy. Now you slap the condenser and dryinig tube on top of the reaction flask and reflux for three hours. After that, let it cool down to room temperature. Then, since all the oil will be sitting at the bottom of the flask, you decant as much of the water as possible, add fresh water, stir, decant again. Do this three times to remove any traces of sulfuric acid left in the oil. Now we want to get our MDP-2-P out of the oil. This is where the sodium bisulfite comes in. Dissolve as much sodium bisulfite as will dissolve in a given amount of water. This makes a saturated solution. Now add the oil to this solution and stir for 30 minutes. The temperature of the reaction will rise and a big mass of crystals will form. These crystals which will look a lot like chicken fat are your MDP2P. Let the solution cool then seperate the crystals from the solution by vacuum filtration. Wash with a little clean dH2O, then wash with a couple hundred mL of ether, DCM, or benzene. Scrape the crystals into a flask and then add 300mL of 10%HCl solution. Stir for another 30 minutes. The MDP2P is taken up with ether, dried and removed of the solvent to give pure MD-P2P.
That method uses really easy to get chemicals but is quite tedious. I will add the most popular method of making MD-P2P, named the wacker oxidation method later, actually it will be a variation of the commonly used wacker oxidation method that blows the original one that everyone is still using on the streets, away. For now I feel like getting into how to make X out of that MD-P2P, it's really easy, you'll shit your pants when you read this next section.
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Making X out of MD-P2P is much easier then making MD-P2P from safrole. The following method is the most common street method for making X, and there is a reason for it. If you have read up on any street drug chemistry or hung out with Outlaw Motorcycle Gang members you may already be familiar with this method, as it is the same method they use to make crank.
It is so great because it uses ordinary household foil. The yeild is a little low at 50-60%, but hey you are reacting your MD-P2P with aluminum foil you can buy at the grocery store, what do you expect. It doesn't exactly use JUST aluminum foil as is, it uses amalgamated aluminum which is easy to make out of aluminum foil, by reacting it with mercuric chloride. Getting the mercuric chloride may proove to be a bitch as it is a very dangerous chemical but you don't need hardly any of it, so your small order of it should slip by unquestioned when you are buying chemicals. If you happen to not be able to buy it, there are a couple ways to make it. One is to obtain mercury which should be pretty easy and obtain some chlorine gas and react the two. The other way is to try and get ahold of some mercuric sulfate and sublime a mixture of it and common salt. mercuric sulfate also seems like it would be a bitch to get, but looking at the MSDSes doesn't appear to be quite as dangerous as the mercuric chloride, but maybe it is the same or more dangerous, I only skimmed the sheets, so I dunno. I'd try buying it straight up first since you don't need that much, then I'd try getting some mercury and chlorine gas since you should be able to get both of those. I don't know exactly how to do this reaction though, looks like I'll be hitting the library, but as I said before from what I've read getting some mercuric chloride should be no problem.
Now this technique with just the amalgamated aluminum makes MDA, this is X but without the methyl group on the nitrogen atom. Lets delve into what exactly the extra methyl group does for you, and you can decide for yourself whether or not its worth the trouble of throwing it on there. MDA and amphetamine are the easiest to make, involve the least watched chemicals, and are the strongest. MDMA and speed although less strong and shorter lasting, are perceived by many as "better" because the highs they produce are smoother and more pleasant. This is not necessarily true as the degrees of differences between MDA and MDMA or amphetamine and speed are very subjective. Strike goes on to strongly recommend making MDA, and talks about why it is better. Basically the more carbon atoms you slam on the nitrogen atom, the weaker the drug becomes. There is actually MDethylamphetamine which is two carbons attached to the nitrogen atom, and it is weaker then MDMA, but still retains some activity. Basically the easy way is to stick with MDA and you will get a stronger longer lasting drug out of it, it just may not be quite as smooth as the MDMA you are used to, on the other hand you wont have to use methylamine to make it, and methylamine is an extremely watched chemical that can get you in big big trouble.
Unfortunatly the method of making MDA with AlHg sucks ass, but a brilliant chemist named Ritter came up with a new method of making MDMA without th insidious methylamine. This is what I will share with you. It uses nitromethane instead of methylamine. So now our reacting chemicals shall be:
MD-P2P
AlHg
Nitromethane(MeNO2)
Where do you find Nitromethane, easy just go down to your local drag strip or auto parts store and pick up a gallon or two for doping your high performance car's fuel. It's also available up to 40% pure in RC model fuels. If you are using the RC model fuel you will have to fractionally distill the nitromethane out of the mixture, it has a bp of 101 degrees C.
Set up a 2 liter two or three-neck flask with an addition funnel and a reflux condenser and provide with a heat source. Not much heat is needed here so a water bath might help keep the temperature down. Stuff 55 grams of one-inch squares of aluminum foil into the flask. Now something that must be mentioned is that you do NOT want to use the thin crappy food grade aluminum foil, that will react too fast and could cause an explosion. You want that thick aluminum foil you use to smoke heroin off of, you know what I'm talking about. The best foil is available in 4"x4" sheets 0.04mm thick, neatly separated from each other with a sheet of tissue paper. This foil is used for sealing flasks. If you don't have access to this wonderful foil, then just use the heroin smoking heavy-duty foil, just not the food grade cheap stuff. Remember to keep a close eye on the reaction rate.
Anywho, fill the seperatory funnel with 50 grams of MDP2P and 50grams or 39mL nitromethane dissolved in 200mL methanol. In another 1 liter vessel add 1.5g HgCl2 to a liter of methanol and allow all solids to dissolve. Very carefully, as I mentioned before HgCl2 is deadly poisonous, use your hood, gas mask, biosuit, everything to protect yo ass, pour the methanolic solution of HgCl2 onto the aluminum foil pieces in the flask and stand back and watch the magic begin. After about 5-10 minutes the bubbling should be sufficient and you may start adding the methanolic mixture of nitromethane and MDP2P drop by drop from the seperatory funnel. As time progresses, the reaction may heat up to the point of boiling and refluxing of the alcohol will occur. This is no problem as the 65 degree C boiling point of methanol is perfect for this reaction. The addition should take roughly one hour and the mixture should be allowed to react for at least 4-6 hours after or until all pieces of aluminum are reacted into a gray suspension. Temperature control needs to be addressed here. If the reaction proceeds under ideal conditions, it will run exactly as described above. If not, and more commonly, the reaction will start to slow down halfway through requiring external heating to maintain a good reaction rate. If things are going badly (no not assuming you blew up, that's if things are going really really badly), an addition of another gram of HgCl2 in methanol solution added to the mix will kick it back in. The next step is the easy part but it must be done right as you want your final product to have NO mercury contamination. Mercury is bad and that's why the HgCl2 may be a bitch to find. Well mercury can be good, hell it can be great, but it's bad for you, and that's why you want to get rid of it in this step. Mix about 1.5 or 2 liters of 35% NaOH soluton and allow to cool. Slowly add the gray aluminum gook produced in the first reaction to the NaOH solution and pour into a large seperatory funnel. Two distinct layers will appear after sitting for maybe an hour, the top being a reddish alcoholic solution of product and the bottom garbage NaOH/Al(OH)3. Simply separate off the garbage bottom layer and discard. Don't worry there's no product tied up in it, and remember that no filtration is needed anywhere in this recovery process compared to other synths out there. Take the top layer and evaporate off the methanol to give an amazing yield of impure amine and a little bit of water. But we are not done yet, there is still the mercury salts in the mix. We must get rid of them, or you are a bad cook. You can poision your customers all you want, but I'm gonna tell you how to do this right, so don't blame me if you skip this last important step. Dissolve the crude product in about a liter of toluene (toluene is watched so be careful, a hardware store may sell it even though it is watched so look around. If you can't find it, as you probably can't, the DEA hates toluene, you can make it out of Benzene by reacting the benzene with CH3Cl in the presence of AlCl3. I'll have to look more in depth for further info on this reaction. I'm not finding shit on the net about it besides what I've told you so I'll have to hit a sci journal. I'll probably be posting a better technique using a higher powered catalyst later anyways so you may not even need to worry about finding the HgCl2 or toluene. For now what you see is what you get). Allow me to finish, The crude product has been dissolved in toluene, now wash the product/toluene with several portions of water in a seperatory funnel and finally with saturated NaCl solution. Dry the toluene with about 50g anhydrous MgSO4. You make the anhydrous MgSO4 by heating drug store epsom salts in the oven at 400 degrees F for an hour, cooling, then powdering. After sitting for an hour or until the toluene is no longer cloudy, chill the dried toluene solution of freebase in the freezer and bubble away with HCl gas to yeild pure MDMA crystals. If they are a little discolored they can be easily cleaned up with an acetone rinse.
There is one more very promising, but very new P2P->amphetamine technique I am going to share with you all, but I will add that later. For now I have completly outlined one of the many ways you can fully synthesize X. Remember don't be afraid to ask questions about anything I covered, I wrote this for YOU.