A Guide to Synthesizing Amphetamines in the age of Chemical Bans
-----------NEW GUIDE BULLITIAN---------------
I have a rare treat for you guys, it's an E-book that is a MUST READ for anyone actually planning on starting up a clandestine laboratory. I will offer it for download off my webserver. Eh, on second that that is a bad idea, because if authorities who will no doubt be interested in my guide, get ahold of my domain they can easily find out who I am and even my address and phone number, so I gotta find another way to host this file. If any of you have webhosting and would like to serve my file, let me know. But reading Jack B Nimble's book has made me rethink some of the things I have said here. Him and I agree on most things, except for obtaining equiptment. He recommends using clandestine/built equiptment for anything you can, unlike me who says buy laboratory grade equiptment when possible. The truth is there is probably a happy medium. He claims even pyrex erlynmeyer flasks are watched, and tho they may be, I doubt they are heavily watched. So truth be told, you are probably aiming for a happy medium of purchased laboratory equiptment and built equiptment. I gotta go for a few hours, I'll talk more when I get back.
Two things, first of all I put in a speil about how you should always be using distilled water, never tap water in your reactions. Sure you can have tap water running through your condensor, but don't be making a solution with tap water or anything.
Next a lightbulb went off in my head saying that I never did check and make sure that all the solvents I'm having you people use are OTC or not, so beware, you may have to actually hit a chemical supply store for some solvents, or do a little research yourself and choose wise substitutes for non-OTC solvents. If someone wanted to help out tho, I'm way swamped writing the rest of the guide to check and see what solvents I mention you can buy at a hardware store etc. So if someone else was really interested in this guide and wanted to help out, they could skim through the guide, make a list of solvents I make you guys use, and figure out which ones are available in really high percentages in products you can buy at a store. If I used an abbreviation, like DMSO or DCM, and didn't say what the unabbreivated name is, which wouldn't surprise me, if you google the abbrivation and solvent google will probably tell you what it is, but if that doesn't work just ask me. I'll have no problems answering any questions, especially one that is being asked to help the guide.
Oh yeah, one last thing that shoul d be mentioned, MSDS sheets are your best friend. They are available freely online for almost any chemical. Just google MSDS and a chemical name and MSDS sheets on the chemical will pop up giving you all the basic information you need to know about the chemical, and most importantly all the saftey considerations you should observe when working with the chemical, like what not to store it by, what to do if you accidntly breathe it, etc.
The Wikipedia also has great sections on many different chemicals, so try a wikipedia search on a chemical for more info on it too.
Okay class, first of all I have to start with the disclaimer: I have never, nor will ever attempt any of the following procedures, and I strongly recommend you never do to. This info is posted purly for educational purposes and I stand at no fault for the consequences of the actions of anyone attempting the procedures described herein.
That out of the way, lets have some fun! This is going to be a modular guide, basically there are lots of steps that have to be taken to successfully create methamphetamines in the age of chemical bans, because you have to make most of the chemicals you use for the final reaction. Hell you have to make some of the chemicals for the intermediate reactions. So basically if a person were wise and going about attempting to make methamphetamine HCl, they would probably not do a little of each step in chronological order, but would rather spend lots of time making each banned chemical, and stockpiling it (a wise person would probably stockpile it in a very hidden spot. Keeping your extra chemicals in a storage facility for instance would probably be a good idea, make sure you read the MSDS sheets on the chemicals you buy and make, as I will not be describing the storage conditions and/or dangers of the chemicals for the most part, it is readily available from MSDS databases online for free). And once you have a lot of each chemical, you just use them until you run out of one, make a bunch more of the one, and do the neccisary reactions until you run out of another, make a bunch of it, and keep going. Some of the chemicals that are banned and you will be manufacturing (so it would be a good idea to not get caught with any of these) are:
methylamine
Iodine crystals
levo-phenylacetylcarbinol
phosphorus acid
l-Ephedrine
Benzaldehyde (you wont be making this, and you'll be getting it out of a common grocery store product of which it makes up like 97% or so, but keep in mind that it is a banned chemical so be careful with it).
Benzaldehyde is a great example, many chemicals you will buy from stores, like Toulene, Sulfuric Acid, acetone, and nitroethane are listed chemicals. They are available unwatched and OTC disguised as common household products, often pure. But you still have to remember that you are possessing a listed chemical and you gotta be careful not to get caught with the wrong combinations of chemicals, do your buying smart, don't buy chemicals at the same time that react with each other for a reaction you are doing
buy a chemical for this reaction, and that reaction, and maybe even that other reaction at the same time.
But that was a lot of common sense, now I will start with things that arn't common sense.
As I said, this guide is modular, it will appear to be in no particular order, and that's cause there really isn't much of an order to go through other then to make sure that you have everything you need before you perform a reaction. I will explain where to get chemicals you need in each seperate synthasis, and if you get a chemical by making it I will mention it, and that means you gotta scroll about the guide and find that chemical and make sure that plenty of it is made before you attempt to do the synthesis that you were reading.
I decided to further modularize this guide by making it multi-threaded. Basically there will be threads on making clandestine labs and making and obtaining the equiptment and a thread on laboratory techniques. That way this post wont be so intimidatingly long, and I can throw in other drug syntheses as I see fit. I'm already planning on making a thread devoted to making X and "prope dope" by using the (MD)P2P reaction. If it turns out that there are a lot of shared chemicals you have to make between the various syntheses, don't be surprised if you see yet another thread on making useful chemicals for drug syntheses.
Now the Chemical synthesis section. I will only explain how to construct an apparatus ONCE. To accomplish this, all the explanations on how to make setups that you see over and over again are after the chemical synthesis section. So like when I say "reflux" or "distill" or "vacuum filter" "wash" "dry" etc etc etc, just look after the chemical synthesis section in the section on common procedures.
IMPORTANT NOTE! You will be using distilled water whenever I say "water." You buy it by the gallon at the grocery store, tap water is NOT an option, it has way too many contaminants and other chemicals that will really fuck up your chi.
---Chemical Synthesis Section ---
Contents:
1. The main reaction!
2. Brewing l-PAC
3. l-PAC into l-Ephedrine using aluminum foil or a microwave oven.
4. extracting phosphorus acid
5.Making Iodine Crystals from Iodine 7% Tincture
6. Benzaldehyde
7. Methylamine
--- The main reaction! d-methamphetamine HCl from l-Ephedrine HCl, Phosphrous acid, and Iodine ---
In a 250mL flask dissolve 25-30g of phosphorus acid in distilled water, then add 24g of Iodine crystals, then place in an oil bath and attach a condenser thus making a reflux. Heat the mixture to 90C, you will see the I2 dissolve and HI will be formed. Keep at 90C for 10-20 minautes. Remove from the oil bath and allow it to cool to room temperature. Remove the condenser and add 20g of the Ephedrine HCl and a boiling stone or two, then put the condenser back on and put it back in the oil bath raising the temperature to 130-150C, for the rest of the reaction never allow it to go above 180C. Maintain its heat for 12 hours, make sure you check on it regularly.
A normal cook will just crystalize the meth right out of this, but we are not normal cooks, we actually work up our products to purity. To accomplish this dilute by adding an equal volume of water. If you just used tap water you dun fucked up, I told you when I say water I mean distilled, always. Wash with hot naptha 2 times. Add an equal volume of naptha as the reaction fluid, and prepare a 25% lye solution (sodium hydroxide). You may have even wanted to make the lye solution a while ago, like during that 12 hour reflux because you can't use it until all the NaOH is dissolved and it is cooled in a freezer before using it. Add the lye solution VERY slowly, like 5mL at a time, keep adding more and more lye solution until you get that pH up to 14.
--Brewing levo-phenylacetylcarbinol from benzaldehyde and yeast--
Okay the basic reaction in this is an enzyme reaction with the enzyme in yeast: Pyruvate Decarboxylase. Basically the reaction is you have a big bunch of yeast and yeast-food so it the yeast has something to munch on. You throw the Benzaldehyde and a couple other extremely common chemicals into the bucket of yeast, the PDC enzyme in the yeast starts eating the benzaldehyde and spitting out l-PAC, pretty simple. Now I'll explain it more in depth. Lots of research has been put into this biotransformation, I have personally read 20-30 or so page scientific journal articles just on ways to try and produce the highest yeild. The highest yeild is obtained by actually purifing the PDC enzyme and using it alone to transform the benzaldehyde, without any of yeast's other enzymes getting in the way, but that's a bit tricky and will be covered in a whole different chapter.
First you will need to get ahold of the Candida Utilis strain of yeast. Yes, you can use ordinary baker's yeast from the grocery store, I believe that is S. Cerevasiae or something like that strain, but C. Utilis works best from all the many studies they have done. It isn't hard to get C. Utilis yeast, it really isn't hard to get just about any strain of yeast you want, you just have to look around. Once you've bought it if you read up on brewing and such you can learn how to grow your yeast and never have to buy it again too, but I'm not going to cover that here. Next you buy sugar beets, and make extract by crushing, grinding, pressing, and filtering the sugar beets. You can use all sorts of different things to feed the yeast, but sugar beet extract apperently works best. Later I may delve into some of the other substrates you can use out of one of my books. Anyways, get 4.5 gallons of beet extract, and get some brewer's sugar, and add a good 5 lbs or so of brewer's sugar to the beet extract. Of course keep this all in a 5 gallon bucket, or a bigger bucket if needed. Next add yeast, the more yeast you add, the faster the reaction will happen, but yeast is expensive if you are buying it, so once again it is encouraged that you start a little yeast farm and grow lots of yeast. That way you'll have lots to throw in the bucket. You can put in up to as much yeast as you put in brewer's sugar (in weight).
After 10 hours or so, add benzaldehyde to the bucket. Benzaldehyde is bitter almond oil, you just have to make sure it is bitter almond oil, not sweet almond oil, and FFPA (Free From Prusaic Acid). FFPA bitter almond oil is very expensive, so I am probably gonna throw a benzaldehyde synth in here somewhere. Before you become completely turned off by the cost of the oil, you have to look at how much product you can produce with it. It's density is 1.05 g/cc at 20 degrees C. You buy a 0.5 fluid ounce bottle for about 30 bux hypothetically. half an ounce is 14.7 cc which means you have 15.43 grams of benzaldehyde for 30 bucks. That will make about `0.8 grams of l-pac which will make about 3.88 grams of ephedrine. 3.88 grams of ephedrine will ideally make you like an 8 ball or so of methamphetamine, so your main precursor for the methamphetamine costs about $30 an 8 ball. That's if you buy in crappy little half ounces, if you buy in more bulk then the price would drop a bit. But still for anyone who is still whiney about bitter almond oil being so expensive, I'll try and post a good OTC benzaldehyde synth.
Anyways, the more benzaldehyde you add, the more l-PAC you will get out. Ideally you will put about 60 mL in there. That may not seem like much, but it is like 62 or so grams! Once you add the benzaldehyde, store in a cool dark place away from sunlight.
Once the reaction is complete, this could take days to weeks to even months depending on how much yeast you put in there. Lots of yeast and your probably good after a few days. I'm getting most of the info I'm using for this from one source and it's not the best source on the matter but it is the easiest to understand, I will come back and revise this later with more accurate details about how long it should take and how much yeast you should put in, but for now you'll just have to experiment. This process reaches a peak and after that point another enzyme in the yeast starts to break down the l-PAC into benzyl alcohol, that's bad. So finding the peak time just when all the benzaldehyde has been converted is key. I'll be able to give you a better idea of when that is when I get some of my other documents. I'm trying to pump out the first draft quick tho.
This document I'm using as my main source has ways to seperate out the l-PAC and they are all good and dandy, but I've got a much easier way to seperate it. For your own knowledge I will explain that this guide says to do an extraction with a non-polar solvent, preferably acetone. Now I don't know how many different ketones are created in this biotransformation process, but my guess is there arn't a whole heck of a lot other then your l-PAC. So you can be sneaky and use sodium bisulfite (bisulfite not bisulfate) to crystalize a ketone out of a mixture. Go ahead and do a really sloppy simple extraction just to get some of the crap out of the way. Make a saturated solution by dissolving as much sodium bisulfite as you can in water. Then add the mixture containing l-pac to it. Stir for 30 minautes and a bunch of crystals that look like chicken fat should form. Vacuum filter the crystals out of the mixture then wash the crystals with some water and then DCM or benzene. Make a 10% HCl solution and put it in a flask with the crystals. stir for 30 minutes. That will bust the sodium bisulfite right off the ketone and then you take the l-PAC up in a solvent like ether, dry, and remove the solvent to yeild what should be pure l-PAC.
The above method should work for seperating out the l-PAC as it appears to be a ketone to me, and this method works on phenyl-2-propanone a very similar ketone, but l-PAC is kinda weird in that it is an acetoin which will make it behaive differently from a regular ketone, but not different enough to effect this process methinks.
Update!- I have read through some of my other sources and am almost ready to post an alternative brewing strategy which may or may not be better, but is the result of lots of labratory research, so I'm gonna assume it's better. Here it is:
I'm not going to cover the basics of brewing here, I'm going to save that for the techniques section where I will devote a chapter just to brewing techniques like raising your yeast, extracting your yeast, feeding your yeast in a fermentation. Here is the specific stuff you need to apply to a standard fermentation that will be outlined in the techniques section. If you can't wait long enough for me to post the technique, just read directly above here and kinda fill in the blanks with what that guy did to brew l-pac.
First off we are going to be using the cheapest and easiest to get ahold of strain of yeast possible because the strain doesn't really matter that much. The above article may be correct and the C. Utilis strain may be the best for the job, but it is not so much better that you need to go through tons of extra trouble for it. You can walk into a grocery store and buy Active Dry Yeast really cheap, which is the strain Saccharomryces cerevisiae for the record. When I say "yeast" or "yeast extract" I'm assuming you are using that strain in this article, but it really shouldn't matter what strain you are using, this one is just the easiest and cheapest to get. Next thing you need to know is that you will be using 0.1mL of everclear per gram of yeast you use (the book just says yeast, but I am assuming they are talking about yeast extract and not wet yeast you just took out of a culture, I could be wrong tho but I doubt it) Use 1mL water for every gram of yeast you use. You will determine the amount of yeast used (and thus the amount of water and everclear) based on how much benzaldehyde you wish to transform. The ideal ratio is 5 grams of yeast for every millimole of benzaldehyde used. A millimole of benzaldehyde is a mere 0.106g of benzaldehyde. You will definetly want to be producing your own yeast or it will get expensive fast, luckily yeast is a living thing that grows and reproduces itself as long as its needs are met, so it isn't some ultra-hard synthesis to produce your own yeast. You will keep this fermentation at as close to 4C in temperature as you can, and you will let it ferment the benzaldehyde for 24 hours before extracting the l-PAC out of the mix, any longer then 24 hours and you are just making by-products. I read in one of the many articles I've read on this subject that these aromatic compounds, particularly benzaldehyde if I remember correctly kill the yeast, so you might not be able to recycle a whole heck of a lot of yeast, but it's worth a shot recycling the fermentation medium after you pull the l-pac out, that's an awful lot of yeat to be using, I'm gonna check one of the other scientific journal articles I have on this computer and see if this book is right about using that much yeast, but adding the everclear and water, and keeping the fermentation at 4C is right on the money. Lots of research has shown that ethanol increases yeilds of l-pac and so does keeping it at 4C.
Anyways, you will be removing the l-pac via sodium bisulfite as explained above (remember -ite NOT -ate). I just remembered something that will make things a little bit trickier in this aspect: The same lovely enzyme that makes us l-pac also makes plain acetoin out of pyruvate and acetaldehyde. Acetoin is just like l-pac with a methyl group where the benzene ring belongs, which in english means they are pretty similar. This means seperating them from each other will proove difficult, acetoin is a ketone and I am assuming it will crystalize with the sodium bisulfite as well. I will figure out how to seperate the acetoin from the l-pac tho.
--- l-PAC into l-Ephedrine using aluminum foil or a microwave oven ---
There are many many many ways to make l-PAC into l-Ephedrine because if you have ever heard of P2P or prope dope, well this reaction is exactly the same as any reaction to make phenyl-2-propanone into methamphetamine. The difference is that there is an alcohol on one of the carbons, and stereoisomerically pure. I will explain the significance of stereoisomers in the techneques section.
Although there are so many ways of performing this reaction, there were two ways that really caught my eye because of thier simplicity and the OTC nature of thier chemicals. First I will be covering the reaction of l-PAC with activated aluminum and methylamine or nitromethane. You can choose between methylamine and nitromethane, but as you will read in the methylamine section, it is watched like a hawk, and you can buy nitromethane as racing fuel. It's not a tough choice, but I thought I'd throw it out there since people have been doing this reaction with methylamine for years, and the nitromethane thing is kinda new. I will assume you have chosen to go the nitromethane route though.
Basically you need heavy duty aluminum foil, you can NOT use the thin foodservice foil, it will react too quickly and probably cause an explosion. The heavier duty the foil, the smoother your reaction will go. You can use heavy duty reynold's wrap and keep a close eye on the reaction, or use something really thick like a cut up pie tin made out of aluminum. Cut this aluminum into 1 inch squares and cut out 55 grams of them. Stuff the squares into a flask and put a condensor on it to make a common reflux setup. This book calls for a two or three necked flask with a seperatory funnel on one neck and condensor on the other. If you can obtain a two or three necked flask by all means do this reaction with it, but for those who are too cheap to buy an expensive three necked flask, you can ghetto rig things by removing the funnel with drying agent from the top of the condensor and adding your chemicals down the condensor with a seperatory funnel. That's how I'd do it anyways.
Obtain 1.5g of mercuric chloride, mercuric chloride is kinda a bitch to get nowadays, they are really trying to discourage the sale of mercury based products OTC since mercury is poisonous. You may still be able to get it at a photography supply store, mercuric chloride is used as a brightener in photography, and a damn good one apperently. As you can see, you only need a little bit of it to activate the aluminum, and I'm looking into whether or not it is feasible to recycle your mercury after the reaction is completed so hopefully you will only have to buy the HgCl2 once or twice. Anywho, dissolve the 1.5g of mercuric chloride in 1L of methanol. Be careful when dealing with any mercury containing compound in chemistry, mercury is poisonous. Also in a seperatory funnel dissolve about 50 grams of l-PAC and 50 grams of nitromethane in 200mL of methanol. Methanol is a common solvent you should be able to buy at a hardware store. Once all solids are dissolved, carefully pour the 1L HgCl2 solution into the reaction flask. If it doesn't completly submerge the aluminum foil, add more methanol until it does. It will start bubbling in your reaction flask. After 5-10 minautes you can begin to add the l-PAC/nitromethane solution to the reaction flask drop by drop. The reaction flask will heat up and you may see your solvent start to boil up into the condenser. The addition should take about an hour, and after that you should let the reaction go for about 4-6 hours until all the aluminum is reacted. The reaction may slow down after a while, if it does, use external heating to keep the reaction rate up. If that doesn't work, add another gram of HgCl2 in methanol solution to kickstart the reaction again.
Now you need to isolate your ephedrine. Remember that ephedrine freebase is not stable in the air so you will be crystalizing it to yeild pure ephdedrine HCl crystals. People that go through all the trouble of having a few people buy lots of sudafed from different stores would shit thier pants if they saw you with all your pure ephedrine crystals. Anyways, make about one and a half, two liters of 35% NaOH solution and allow to cool. Slowly add the contents of the reaction flask to the NaOH solution and place this in a large seperatory funnel. After about an hour two layers will form. The top layer is your ephedrine in methanol, the bottom layer is Al(OH)3 in NaOH. Drain this bottom layer, and get rid of it, or try and get the mercury out of it if getting that mercuric chloride is a problem. I havn't researched the mechanism of this reaction enough to be able to tell you whether or not mercury from this reaction is even recyclable or not, but I imagine it is. Next you take that top layer and evaporate off the methanol to yeild ephedrine freebase in some water. But beware there is still some left over mercury in this product, and that is bad. Dissolve the crude product in about a liter of toluene (another common solvent available at the hardware store. It is listed tho so I wouldn't order it from a chemical supply company, definetly get this OTC). Wash with water multiple times in a seperatory funnel and lastly with a saturated NaCl (table salt) solution. Dry the toluene with about 50g of anhydrous MgSO4 made by heating drug store epsom salts in the oven at 400F for an hour, cooling then powdering. Let the toluene sit until it is no longer cloudy. Next chill the dried toluene in a freezer and then you can bubble the HCl gas through the toluene solution to yeild ephedrine crystals. Vacuum filter and you have the DEA's current favorite chemical, without having to do sneaky things and lurp around town.
--Getting phosphorus acid out of fertilizer--
Well I can't explain it any better then this guy, and his writing is clear enough that I don't really have to simplify anything. So I'm just going to copy and paste his document here and give credit:
Swi1phen's Complete OTC H3PO3
you guys really should learn to watch out for turf plant diseases. just a friendly tip.
So im bringing the last few months of experiments to a somewhat compacted conclusion. This felt like the right way to sum it all up...
I do not give sources first of all, but its soo incredibly easy to buy products from like flower shops or turf care specialists...
The product that swiyou or anyone can use must be of the phosphite salt or simply liquid phosphorous acid in solution.
First, we will start with the extraction of potassium phosphite and conversion to phosphorous acid (h3po3).
Once swiyou googles for about an hour, then you will understand what its all about.
Anyways i will assume you have one of the products that will work with this extraction, its very forgiving and very simple.
In a 500ml pyrex beaker pour 200ml of phosphite solution. And 200ml of HCL acid (muriatic is fine). {When scaling up its simply equal amounts
of phosphite solution to HCL.
Stir with wooden spoon for a few seconds to ensure maximum surface area.
Now simply heat the solution on LOW (never should it boil). You will see lots of potassium salt out, when potassium has accumulated quite a bit,
take the pyrex cup. cover with saran wrap and put in freezer. Now when you come back in about 30 minutes lots more K (potassium) has salted
out.
Filter and return liquid to pyrex cup and return to heating and do the process till no more potassium rears its ugly little head.
Not that hard right? Basically simple.
Now when it gets down to the last 50ml pour the liquid into a pyrex evaporation plate to increase surface area.
Start watching very closely, when the phosphorous acid is ready it will be a vicious syrup, when you see this, quickly take off heat, cover
the plate with something air tight.
Leave it in the freezer for a few hours, when you return you will have a waxy solid. That is youre H3PO3. And dispite first beliefs,
the impurities are very very miniscule.
Quickly scrape up with a razor, place in a hdpe bottle with cap and tape it on good!
Thats it! From a gallon of product that is very very legal for homes and gardens, you can get easily a couple hundred grams of phosphorous acid.
---Iodine crystals from Iodine 7% Tincture ---
Iodine 7& Tincture is a common product used in horse care. I found an online horse supply store selling it at about $25/gallon. Of course you wouldn't buy online and will probably pay a little more. The best part about Iodine in this reaction is that it is 100% recycleable if you play your cards right and do a little post reaction work. So you'll only need to this once in theory. Also you can buy 2% Iodine Tincture in little bottles at the grocery store, this will work too but you will pay a lot more for a lot less iodine crystals. The risk is also a lot less carrying home a few bottles of the 2% tincture bought from a couple different grocery stores then hauling home a gallon of the 7% tincture from a horse supply store. Anyways, here is how you take iodine tincture and make iodine crystals out of it, this is using someone else's voice, because they explain it better then I can.
Making The Iodine Crystals
-What You Need-
* 20-Oz Coke Bottle
* 4 Bottles Iodine
* Hydrogen Peroxide
* Muriatic Acid
Take one 20 oz, plastic Coke Bottle and pour 4 Bottles 2% tincture into it.
Add Hydrogen Peroxide to this. Use only 1/2 a bottle of Hydrogen peroxide. After this, take the cap from the gallon jug that the Muriatic acid. Fill it with the acid and pour it in.
(Place in a freezer for at least 30 minutes).
Get a clean mason jar, on top of this place 1 coffee filter and pour the contents of the Iodine + Muriatic Acid + Hydrogen Peroxide mixture into the filter (do it slowly don't over pour) Once you get though with the filtering, there will be a black substance on the filter. (These are iodine crystals)
Dry them by wrapping in more coffee filters till you get a pretty good thick pile around the original filter, place on ground and step on it to get the rest of the liquids off.
Save this for the cook.
I'll come back and add how to recycle the iodine later...
---Benzaldehyde---
I already talked a little bit about benzaldehyde in the chapter on making l-PAC, but here I'm going to go more in depth. As I mentioned benzaldehyde is bitter almond oil. Bitter almond oil is expensive, so we will examine some other ways of obtaining benzaldehyde.
Artificial Almond Essential Oil is benzaldehyde, alcohol, and water. The alcohol and water will be fine in a l-PAC brew so if you find that product for cheaper then the bitter almond oil, you can use it instead. From a little bit of online searching it appears artificial almond flavouring is a lot cheaper then bitter almond oil, but is harder to find. Now if you are a real cheapskate, you can make your own benzaldehyde.
It isn't easy, but you can make your own benzaldehyde by starting with Benzyl Alcohol, a common solvent and photographic developing chemical, or toluene which is also a common solvent and is used as a paint thinner. You have to partially oxidize either chemical to make benzaldehyde. I'm still looking up good OTC techniques of doing this, but one that I remember vaugly involves microwave irridation of benzyl alcohol to benzaldehyde using manganese dioxide (a chemical used in batteries) suspended in silica gel (silica gel is that crap in the little packet that comes with stuff you buy, used to keep it dry.) I'll try to find that synthesis as well as some other good partial oxidations. In the meantime you are stuck using the bitter almond oil or artificial almond extract/flavoring/whatever.
--- Methylamine ---
Methylamine is a heavily watched substance so you wont be buying this. You'll be making ityay! There are quite a few OTC ways to make methylamine so the fact that the DEA loves it almost as much as ergotmine and pill presses shouldn't phase you.
The first way I will describe is a traditional way of making it, which is with formaldehyde and ammonium chloride. First lets talk about the formaldehyde, there are two ways you can get it, you can either buy it the easy way, which could raise some eyebrows, as just 40% (37% by weight) formaldehyde. It is sold as the product formalin and is available in small bottles at pet stores to kill parasites on fish. It is extremely handy to buy it this way because any time I use formaldehyde in a synthesis I call for 40% by volume formaldehyde in water (which is 37% by weight.). But on the con side I don't think you can easily or possibly even safely buy a bunch of formalin. The DEA tends to at least keep an eye on anything that is as useful in making pharmacuticals as formaldehyde. Not to mention what do you say when you buy a bunch of formalin repeatedly, that you have a huge tank of fish and they keep getting sick? No, the solution for a high volume of formaldehyde is to get paraformaldehyde and depolymerize it. Basically what you do is you buy the product MildewCide. It is 91% paraformaldehyde by weight. You can buy lots of it without any suspicion at all. Put the MildewCide in a flask and attach a gas bubbler. Now you get a container of water, if you want to watch the bubbling action it can be glass/pyrex, if you don't like bubbles or have a bubble-phobia, it can be plastic so you don't see them as well, it really doesn't matter. Now I will remind you again that the water should be distilled water, extra contaminants will change the weight of the water and really throw things off. Remember 1L of pure distilled water equals 1Kg. calculate 91% of the weight of the MildewCide you put in the flask, then we do some simple math. Lets say we have 5 grams of MildewCide. That should be 4.55 grams of paraformaldehyde. Now we want 37% of our total weight to be 4.55g, so we divide 4.55 by 0.37 and get that our total weight will be about 12.30g. Now we simply subtract 4.55 from 12.30 and we get 7.75g of water. So we measure out 7.75mL of water to bubble the paraformaldehyde through. You may want to maybe add just 7mL of water in that case because you never know exactly how much over or under the 91% the actual content of paraformaldehyde is in your particular bag of MildewCide, and it would suck to have too much water making your solution under 37%. If your solution is over 37% you can always just add more water, but if it's under, that makes things difficult because formaldehyde has a lower boiling point then water, so you can't really boil water out. You don't have to be right on either, just be as close to 37% as you can get. To measure your solution's formaldehyde %, measure the volume. Hopefully you have written down, or remember how much water you put in. Divide the volume of water by .60 to get the ideal volume of the solution. If the actual volume of the solution is under, add water until it is the ideal volume. Oh yeah, I forgot to tell you how to get the formaldehyde into the water. Heat the flask with the MildewCide to between 180-200C using a temperature regulator or oil bath. The paraformaldehyde will depolymerize making formaldehyde gas. Luckily formaldehyde is extremely soluble in water, so as long as you have your gas bubbler submerged in the water, it'll make a solution. Simply do this until the bubbler stops bubbling.
Next thing you need is the ammonium chloride. You can buy it in blocks at the hardware store for cleaning the tip of a soldering iron.
okay, here is the methylamine synthesis: In the reaction flask of a simple distillation setup put 2000g of 40% formaldehyde (formalin) and 1000g of ammonium chloride. Slowly heat the mixture to 104C, the ammonium chloride will dissolve and the solution will be a bright, clear golden color. CO2 bubbles will be evolved and as the solution nears 100C a bunch of stuff will start to come over. Hold the temperature at exactly 104-105C for 4-5 hours, any hotter and there will be product loss, so if the temperature is to go out of bounds, make sure it gets too cold instead of too hot.
The stuff that came over is crap, what you are interested in is what is left in the reaction flask. As the solution cools a big mass of unreacted ammonium chloride will form. Remove this with vacuum filtration. You can save these ammonium chloride crystals for the next time you perform this reaction, or any other reactions you happen to be doing that require it. Now you will place it back in the reaction flask and go ahead and hook up your vacuum pump. This time temperature is not a huge issue, because methylamine HCl has a melting point of 230C, it wont be boiling over anytime soon. Boil out crap at whatever temperature is neccisary, sometimes thre will be yet more ammonium chloride crystals forming, vacuum filter them out as soon as they form and continue to vacuum distill the solution. Sometimes you have to repeat this process a couple times to get all the ammonium chloride crystals out of the solution. Once you have gotten all the ammonium chloride out, you distill once more and once everything that will boil has boiled, you will be left with methylamine HCl crystals in the reaction flask. If stuff completly stops coming over and there is still no crystals, this means you are over the melting point of the methylamine hcl and you just need to let it cool down and poof your crystals will form. This last scenerio is extremely possible if you have a good vacuum and really get that melting point down.
The way you know it is methylamine hcl crystals and not ammonium chloride is that the ammonium chloride crystals that you will get out of the solution will be white, tiny, and fuzzy. On the other hand the methylamine hcl crystals are longer, more crystalline and a lot more sparkly. Vacuum filter the solution+methylamine hcl crystals, and put the solution back in the reaction flask and try and squeeze more crystals out of it. Vacuum filter again and you should have a nice filter cake of methylamine hcl crystals. Wash this filter cake with a little chloroform, scrape into a beaker of hot ethanol (everclear is a fine substitute for ethanol, as it is like 95% ethanol or something). Chill the ethanol with the methylamine in it and the methylamine hcl will recrystalize, vacuum filter the crystals out of the chilled everclear and you will have clean crystals!
The second method I will go over is a newer-age method which involves reducing nitromethane to methylamine. This method is also very OTC as nitromethane is racing fuel and can be bought at a auto retailer to put in your gas tank for your high performance engine. There is other chemicals used in a similar manner, so make sure you check beforehand or on the label if it's on there and make sure it's nitromethane. Now my source says to purify the nitromethane through vacuum distillation, but you need a serious vacuum to bring the boiling point down far enough to be safe, remember you are dealing with racing fuel, it will explode! Now, if you are doing the activated aluminum reaction I will outline in the chapter on making ephedrine, you can substitute the nitromethane right in there for the methylamine and never have to touch methylamine, the activated aluminum will reduce the nitromethane into methylamine right there in your reaction flask, the methylamine will grab onto the double bond, then the activated aluminum will reduce the intermediate compound into ephedrine.
For the other reaction, I wouldn't put racing fuel in a microwave, that sounds like a bad idea. So instead we reduce the nitromethane ourselves.
Actually I'm going to save this reduction for the next draft, I'm spending way too much time on methylamine, which you wont even use if you decide to go the activated aluminum route instead of the microwave route. So check back in a little while after I get more of the guide done if you are interested in using the microwave route and reducing nitromethane to accomplish it. It's really simple actually.
Originally Posted by Ollie Cromwell
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