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Newsgroups: alt.drugs
I believe this will eventually be in the MDMA FAQ (or at least the info
in it will be...):
INTRODUCTION:
All information here is to be used at your own risk. The procedures
documented in this file, if carried out by unlicensed individuals would
violate laws against controlled substances in most countries and could result
in criminal charges being filed. If carried out by individuals unskilled
at chemistry they could result in serious bodily harm.
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.
PRECURSORS:
The following chemicals are some of the more important ones in the
synthesis of MDMA and related chemicals:
O
||
O //\ /\ O //\ /\ O //\ /\\ O //\ /\\ NO2
/ \// \/ H / \// \/ \ / \// \/ \\ / \// \/ \\/
/ | || / | || || / | || | / | || |
CH2 | || CH2 | || || CH2 | || | CH2 | || |
\ | || \ | || CH2 \ | || CH3 \ | || CH3
\ /\\ / \ /\\ / \ /\\ / \ /\\ /
O \\/ O \\/ O \\/ O \\/
piperonal safrole isosafrole beta-nitroisosafrole
O //\ /\ O O //\ /\ Br
/ \// \/ \// / \// \/ \/
/ | || | / | || |
CH2 | || | CH2 | || |
\ | || CH3 \ | || CH3
\ /\\ / \ /\\ /
O \\/ O \\/
MDP-2-P 3,4-methylenedioxy-
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 MDMA in clandestine labs.
SYNTHETIC ROUTES:
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 most common synthetic routes for production of MDA, MDMA, MDE (MDEA),
and MDOH 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. This latter procedure 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:
1. Sodium Cyanoborohydride
2. Aluminum Amalgam
3. Sodium Borohydride
4. Raney Nickel Catalysis
5. Leukart Reaction via N-formyl-MDA
6. Leukart Reaction via N-methyl-N-formyl-MDA
The sodium cyanoborohydride method is probably the one most attractive to
clandestine chemists. From the Dal Cason reference:
"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. 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. 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. 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.
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. 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.
Methylamine can be synthesized through hydrolyzing N-methylacetamide via
refluxing it with concentrated HCl. This leaves water, methylamine and acetic
acid, boil of the water, and strip the acetic acid off with a vacuum pump
and what's left is the methylamine. 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.
SUMMARY:
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]