MDMA ("Ecstasy") is a semi-synthetic compound which can be made relatively easily from available precursors. Synthesis instructions exist which can be followed by an amateur with very little knowledge of chemistry. However, people with less than 2 years of college chemistry experience would probably not be capable of sucessfully synthesizing MDMA, and would either botch it in the best case or kill themselves in the worst case. For those interested in the techniques involved in synthesizing MDMA, a good book for self-learning is the following:
Zubrick, James W. "The Organic Chem Lab Survival Manual: A Students Guide to Techniques." ISBN #0471575046. Wiley John&Sons Inc. 3rd ed.It is recommended that this book should be supplemented with at *least* one more of the 'dry' and technical O-Chem lab manuals available at any college bookstore. It is not recommend that the information from these books or herein this file be used to synthesize MDMA for the previously stated reasons. Knowledge, however, is not (yet) illegal.
Also, it has been my perception that when the availability of clean MDMA is reduced, the freqeuncy of adulterated and substituted MDMA increases with a corresponding increase in adverse reactions. With high availability of clean MDMA, frequency of substitution is reduced.
Precursors
The following chemicals are some of the more important ones in the
synthesis of MDMA and related chemicals:
O
||
O //\ /\ O //\ /\ O //\ /\\
/ \// \/ H / \// \/ \ / \// \/ \\
/ | || / | || || / | || |
CH2 | || CH2 | || || CH2 | || |
\ | || \ | || CH2 \ | || CH3
\ /\\ / \ /\\ / \ /\\ /
O \\/ O \\/ O \\/
piperonal safrole isosafrole
O //\ /\\ NO2 O //\ /\ Br O //\ /\ O
/ \// \/ \\/ / \// \/ \/ / \// \/ \//
/ | || | / | || | / | || |
CH2 | || | CH2 | || | CH2 | || |
\ | || CH3 \ | || CH3 \ | || CH3
\ /\\ / \ /\\ / \ /\\ /
O \\/ O \\/ O \\/
beta-nitroisosafrole 3,4-methylenedioxy- MDP-2-P
phenyl-2-bromopropane
safrole: 3,4-methylenedioxyallylbenzene,
1-(3,4-methylenedioxyphenyl)-2-propene
isosafrole: 3,4-methylenedioxypropenylbenzene,
1-(3,4-methylenedioxyphenyl)-1-propene
MDP-2-P: 3,4-methylenedioxyphenyl-2-propanone,
3,4-methylenedioxyphenylacetone,
3,4-methylenedioxybenzyl methyl ketone,
piperonylacetone
piperonal: 3,4-methylenedioxybenzaldehyde,
heliotropin
beta-nitroisosafrole: 3,4-methylenedioxyphenyl-2-nitropropene
safrole, isosafrole, MDP-2-P, piperonal and beta-nitroisosafrole are the
most commonly found precursors to methoxylated amphetamines in clandestine
labs. Safrole and isosafrole are typically found as precursors to MDP-2-P
while piperonal is typically found as a precursor to beta-nitroisosafrole.It is not at all feasible to synthesize MDMA from amphetamine or methamphetamine or related chemicals which do not have the methylenedioxyphenyl ring. Likewise, 3,4-dihydroxyphenyl compounds aren't much better suited for precursors.
Synthetic Routes
The synthetic routes for MDA, MDMA, MDE, MDOH, etc are all fairly similar
and in many cases differ only by the subtitution of a suitable chemical for
methylamine or N-methylformamide. Some of the routes are similar to those
that can be taken to synthesize amphetamine and methamphetamine, although
there are differences (i.e. the Ritter reaction does not work for
methylenedioxyamphetamines.) For an overview of MDMA synthetic routes it is
suggested that the readers familiarize themselves very thoroughly with the
following reference:
Dal Cason-TA. "An Evaluation of the Potential for Clandestine Manufacture of 3,4-Methylenedioxyamphetamine (MDA) Analogs and Homologs." Journal of Forensic Sciences. Vol 35(3):675-697. May 1990.The easiest synthetic routes for production of methylenedioxyamphetamines are from the precursor MDP-2-P. To get MDP-2-P first a natural source of safrole is acquired. Safrole can be extracted from sassafras oil, nutmeg oil, or several other sources which have been abundantly documented in Chemical Abstracts over the years. The safrole is then easily isomerized into isosafrole when heated with NaOH or KOH. The isosafrole is then oxidized into MDP-2-P. The synthesis of isosafrole into MDP-2-P has been most clearly presented in Phenethylamines I Have Known and Loved by Alexander Shulgin under synthesis #109 (MDMA). The synthesis of MDP-2-P from isosafrole will require the use of a vacuum pump to evaporate the solvent from the final product in vacuo. An aspirator will not, unfortunately, be sufficient.
Once the MDP-2-P is synthesized there are several synthetic routes which can be taken:
"It requires no knowledge of chemistry, has a wide applicability, offers little chance of failure, produces good yields, does not require expensive chemical apparatus or glassware, and uses currently available (and easily synthesized) precursors"The aluminum amalgam synthesis is often used but has a slightly higher risk of failure and is not as versatile. It is, however, attractive in that aluminum foil is not likely to become difficult to acquire at any time in the near future, while sodium cyanoborohydride could be placed under tighter control. The Raney Ni synthesis is more dangerous and requires special equipment to be done right (although this scheme is used in a significant number of clandestine labs). The sodium borohydride requires harsher conditions for the chemicals (ie. reflux) than sodium cyanoborohydride or aluminum amalgam and produces lower yields. The Leukart reaction is 2-step with lower yields and requires chemical apparatus.
There are also two synthetic methods which proceed directly from safrole rather than through isosafrole. The first is the Ritter reaction which goes through the intermediate N-acetyl-MDA. The Ritter reaction is time-consuming, requires a degree of laboratory skill and produces poor yields. (It is actually somewhat likely that this method is utterly useless for methylenedioxyamphetamines.) The other method uses HBr to produce 3,4-methylenedioxyphenyl-2-bromopropane which is then converted into MDA or MDMA. This scheme produces poor yields, and Dal Cason referenced the australian journal ANALOG where a hazard had been documented. It is, however, attractive for its sheer simplicity. It requires no specialized chem equipment or reagents at all.
Beta-nitroisosafrole is a less used precursor, but there is a large literature on the synthesis and reduction of nitro alkenes. This synthetic route isn't as popular due to the easier availability of precursors for MDP-2-P, and it also results in MDA which must then be further processed to give MDMA or any other N-alkyl homolog of MDA. This approach is most often used by those who can easily divert piperonal from legitimate sources. Provided that the precursor is available and MDA is adequate, this becomes an attractive synthetic route. There are numerous ways to convert beta-nitroisosafrole to MDA: LiAlH4, AlH3, electrolytic, Na(Hg), BH3 - THF / NaBH4, Raney Ni catalyst, Pd / BaSO4 catalyst, Zn (Hg). Beta-nitroisosafrole, when used, is commonly synthesized from piperonal. Beta-nitroisosafrole can also be used as a precursor for MDP-2-P, but this is not commonly done.
There are other synthetic routes, such as the use of substituted 3,4-methylenedioxycinnamic acid or the construction of alkyenedioxy bridges from dihydroxy compounds. These, however, are typically not used for a variety of reasons (difficulty, multiple-step, special equipment, etc). It is also possible to synthesize N-alkyl derivatives of MDA from MDA (e.g. synthesizing MDMA from MDA) but this is not commonly done in clandestine labs, due to the lack of improvement in profit in the conversion.
Methylamine
Methylamine is a chemical which is technically not a "precursor" to MDMA,
but it is necessary in most of the syntheses. It is also a watched
chemical. A private citizen ordering methylamine from a chemical supply
company would get the undivided attention of the local DEA. This is
particularly true more recently as the media attention surrounding
methcathinone and MDMA have caused the DEA to focus more on enforcing
laws against amphetamine derivatives. Methylamine can be diverted in small
quantities by individuals working in legitimate chemical labs. In some
cases this "diversion" is simply theft. It is not recommended that
any persons engage in this activity, but it remains a common source of
methylamine (along with many other chemicals).
Methylamine can be synthesized through hydrolyzing N-methylacetamide via refluxing it with concentrated HCl. Dump a gallon of concentrated HCl in a large RB flask, dump in a mole or two of N-methylacamide and reflux the hell out of it for about 2 days. This leaves water, methylamine and acetic acid. Boil off the water, and strip the acetic acid off with a vacuum pump and what's left is the methylamine. Some acetic acid may be left over, but it shouldn't affect the cyanoborohydride reaction.
It can also be synthesized by doing a large hypohalite Hofmann degradation on acetamide with bleach and lye. Heat it up and distill off the water/methylamine from the basic mush and catch it in HCl. Boil off the water/acid distillate and the result is methylamine HCl.
N-methylacetamide is unlikely to be watched, and acetamide is almost certainly not watched. There are other methods of producing methylamine which are perhaps a little more elegant, but for clandestine manufacture these two methods offer much in the way of simplicity and availability of precursors.
Some syntheses use N-methylformamide as an alternative to methylamine, but it is unlikely that there would be any advantage to using it. The 3 syntheses focused on in this file (HBr, cyanoborohydride and aluminum amalgam) all use methylamine.
Secrets of Methamphetamine Manufacturing has both a synthesis of methylamine and a synthesis of N-methylformamide, but i haven't had a chance to peruse the book to comment on them.
oil of sassafras -------> safrole ----------> isosafrole --------> MDP-2-P
(extraction) | (isomerization) (synthesis) |
| |
V V
*1. safrole + HBr *1. sodium cyanoborohydride
2. Ritter reaction *2. aluminum amalgam
3. sodium borohydride
piperonal ------> beta-nitroisosafrole 4. Raney Ni catalyst
(synthesis) | 5. Leukart reaction
|
V
[numerous routes to MDA]
* of interest to aspiring kitchen chemists