Originally posted by Eleusis
The Leukart reaction is so hopeless it's not even funny. Kids, it makes a big mess, is ridiculously temperamental, and the precursors are *not* easily available, nor easily *made*.
Non-metal reductions to amphetamine and methamphetamine have been what might be termed as "fads" in clandestine laboratory synthesis within the United States. In the early and mid 1970's, the Leuckart synthesis, which employs formic acid, was the polular clandestine route to amphetamine and methamphetamine. For whatever reason, this route, which is still very common in Western Europe, lost popularity in the United States by the end of the 1970s. In the early 1980's the hydriodic acid reduction of ephedrine to methamphetamine began increasing in frequency in the Southwestern and Western areas of the United States.
UNCLE FESTER SECRETS OF METH MANUFACTURE 8.5th EDITION
Chapter Two The Leuckardt-Wallach Reaction: An Overview
A good way to produce batches of up to a pound in size is by the Leuckart-Wallach reaction. Back when I was a "producer," this was the method I liked to use, so it has a strong sentimental attachment to me . It tends to be atouchy reaction that if not done correctly will instead give you a bunch of useless red tar. I still love it nonetheless, as it brings back fond memories. Other methods for converting phenyl acetone to meth are covered in Chapters 11 and 12. A variation on the standard Leuckart procedure is very popular in Europe, and is used to make benzedrine from phenylacetone reliably. Their batch sizes using this European variation can work up to over a pound. We'll talk more about this European variation later. A Russian Advance which uses nickel in the mixture as catalyst is also worth checking out, as is aluminum salts in the reaction mixture. The Leuckart-Wallach reaction involves reacting a ketone with two molecules of a formamide to produce the formyl derivative of an amine, which is then hydrolyzed with hydrochloric acid to produce the desired amine. In this case, the reaction is shown in the diagram below. There are several reviews this reaction in the scientific literature, the best of them by Crossley and Moore in the Journal of Organic Chemistry (I 949}. The conditions which favor the production of high yields of fine-quality products are as follows. There should be a small amount of formic acid in the reaction mixture, because it acts as a catalyst. It should be butTe red by the presence of some free methylamine, to prevent the pH of the reaction mixture from falling too low (becoming too acidic). The presence of water in the reaction mixture is to be avoided at all costs, because this really messes up the reaction. It prevents the phenylacetone from dissolving the N-methylformamide, leading to low yields of purple-colored crystal. The recipe I give in a later chapter for making N-methylformamide makes a product which is perfect for this reaction. It is also important that the reaction be done at the lowest temperature at which it will proceed smoothly, and that the heating be continued for as long as the reaction is still going. In this way nearly all the phenylacetone is converted to methamphetamine.
There is one stumbling block in the path of underground chemists: in 1979, the DEA made phenyl acetone illegal to purchase or possess. N-methylformamide is also risky to obtain, although it is not illegal and is used in industries as a solvent.
p2p synthesis
The best catalysts are mono and diammonium acetates made by adding the amine to the freezer-cold Nitroethane slowly under stirring followed by the fridge-cold Benzaldehyde.* GAA may be a small stöchiometric excess. That makes it much easier. B-dehyde should be fresh or get distilled beforehand.
Ratios: 1 mol B-dehyde, 1 mol Nitroethane, 0,05 to 0,2 mol amine enough GAA to neutralize the amine + an extra spritz of it.
As told all monoamines work and most diamines too. Say, propyl, diisopropyl, methyl, dimethyl, ethyl, ethanol, cyclohexyl, ethylene diamine and on and on. Of the over 100 (di)amines you might be able to get one I believe. If not: Get another hobby.
Not only GAA can be used as acid but other organic acids too. Known to work well are formic acid (courtesy hest/HIVE) and benzoic acid (some articel and confirmed). Others will work too - give it a shot and report! Benzoic acid is told to be very soft on the substrates so if one is to condense a substituted sensibel B-dehyde this might be the best choice.
Procedure 1 (recommended): Microwave
- mix and nuke up to 60/70°C - cool down in cold waterbath - repeat - do this as often until SLIGHT discoloration is visible - let cool down slowly at RT and then in the fridge. Crystallisation occurs like magic. For me. If not scratch with glassrod against beaker walls. Seed crystals are best. Safe some and relax.
enhancement P2NP on the pump (that means Büchner + vacuum). Rinse with a little ice-cold anhydrous alcohol (ethyl, methyl IPA...). This adds to the liquid from filtration.
This combined liquid:
- nuke again to 60°C - just once - cool down to RT, fridge etc.
repeat
If you got the timing more or less right there is 70% yield on the first crop, 20% on the second and more comes third maybe fourth (dry weight after recrystallisation from alcohol or petrolether. Use MeOH so you are masochistic or just love to cry a bit from time to time, use IPA if you are not such a painslut)
Of course the broth gets darker every round, doesnt matter after recrystalisation it will be pristine.
The trick is to remove P2NP in time so it stands not in its own way and more can form. The little dilution every time by the rinsing alcohol helps also, it proceeds beautifully.
Drawback: You have to wait for cooling down/crystals and enhancement more often. Plus: The reaction is done in 10 minutes, 5 minutes enhancementing, this 3x makes 45 minutes the rest is watching porn.
Procedure 2: No Microwave - the same just use a heating plate/preheated waterbath - needs longer heating and due to this gives more discoloration and less time for watching porn - in this reaction the microwave is clearly superior to other heating methods
Microwave additional information: - use a not-rotating-table model, a "mode stirrer" type so any possible. - The microwave must be a dedicated one, dedicated to science and progress as you don´t want to use this microwave for food preparation after this. - For batches up to 300ml a low-power model (500-600Watt) is preferred. Bigger batches are better done using several smaller flasks (like 4x 250ml at the same time) then a single big one as the penetration depth of microwaves is limited. - Wide neck Erlenmeyers are preferred, some cotton stuffed loosely into the neck reduces obnoxious fumes to almost zero. - having "nitro" in its name makes nitroethane no explosive per se in special not in solution. Should something happen then not because of the microwaves but because you are an idiot and then the cavity of a microwave is a much better place then a flask on a hotplate near balls or face.
Congratulation! You made it through all these words until the end! Not all hope is lost!
I explained the general theory behind this reaction in Chapter Two. Now, after doing the reactions described in the previous two chapters, the underground chemist has phenylacetone and Nmethylformamide suitable for making methamphetamine. He will want to get going before the chemicals get stale. The tirst thing he does is test the chemicals. He puts 5 ml of phenyl acetone and 10 ml of Nmethylformamide in a clean dry test tube or similar small glass container. Within a few seconds they should mix together entirely. At this point, he may offer a prayer to the chemical god, praising his limitless chemical power and asking that some of this power be allowed to flow through him, the god's High Priest. He may also ask to be delivered from the red tar that can be the result of this reaction. If they do not mix, there is water in the N-methylformamide. In this case, he must distill it again, being more careful this time. Having tested the chemicals, he is ready to proceed with the batch. (However, if the underground chemist was reckless enough to obtain N-methylformamide ready made, he will have to distill it under a vacuum before it can be used in this reaction.) The phenyl acetone he made (about 100ml)is mixed with the N-methyIformamide. The best amount of N-methylformamide to use is about 250 ml, but any amount from 200 to 300 ml will work tine. With 200 ml of N-methylformamide, there are about four molecules of N-methylformamide to one of phenyl acetone. This is the bare minimum. With 300 m!. the ratio is nearly six to one. Any more than this is a waste of N-methylformamide. The best flask for mixing them is a 500 ml round bottom flask. Alier they are mixed, thisflask is set up as shown in Figure 19. The tlask is sitting in an oil bath, to supply even heating to the flask. The oil (once again, Wesson is a good choice) should extend about 2/3 of the way up the side of the flask. A metal bowl makes a good container for this oil bath. This is better than a pan, because it will be important to see into the flask. The fact that the oil will expand when heated is kept in mind when filling the bowl with oil. A thermometer is also needed in the oil bath to follow its temperature.
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