298 lines
15 KiB
Plaintext
298 lines
15 KiB
Plaintext
From: lamontg@u.washington.edu (Lamont Granquist)
|
|
Newsgroups: alt.drugs
|
|
Subject: chemistry: if anyone *ever* asks for a "MDMA recipie" again...
|
|
Date: 23 May 1994 04:56:03 GMT
|
|
Message-ID: <2rpd13$sav@news.u.washington.edu>
|
|
|
|
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]
|
|
|
|
* of interest to aspiring kitchen chemists
|
|
|
|
- the sodium cyanoborohydride method is the preferred method
|
|
- the safrole + HBr route is attractive due to its sheer simplicity
|
|
- the aluminum amalgam route is as useful as cyanoborohydride, but may
|
|
have a slightly higher risk of failure.
|
|
|
|
"POPULAR" LITERATURE:
|
|
|
|
Psychedelic Chemistry: Contains instructions for isomerizing safrole,
|
|
a synthesis of MDP-2-P from isosafrole, and a synthesis which uses the
|
|
Leukart reaction. The synthesis of MDP-2-P is better presented in
|
|
PiHKAL and the Leukart reaction is is not a recommended synthesis. Also,
|
|
please see "ROAD HAZARDS" below, on the dangerous typos in this
|
|
synthesis.
|
|
|
|
Secrets of Methamphetamine Manufacturing: Contains instructions for
|
|
synthesizing MDMA via the safrole + HBr method. This is the simple and
|
|
dirty way to synthesize MDMA. Pay attention to the part where it tells you
|
|
to make sure that you've got all the ether evaporated before placing it
|
|
in the reaction bomb... for your own good. References to the original
|
|
journal articles and Chem Abstracts are included.
|
|
|
|
PiHKAL #100 (MDA): Synthesis of beta-nitroisosafrole from piperonal,
|
|
synthesis of MDA from beta-nitroisosafrole using lithium aluminum
|
|
hydride, synthesis of MDA from MDP-2-P using sodium cyanoborohydride.
|
|
The latter is probably the most useful. Although piperonal is commonly
|
|
used to synthesize beta-nitroisosafrole. LAH is somewhat dangerous.
|
|
|
|
PiHKAL #105 (MDDM): Synthesis of MDDM (N,N-dimethyl-MDA) from MDP-2-P
|
|
using sodium cyanoborohydride. This stuff isn't terribly active, its
|
|
just another example of a sodium cyanoborohydride synthesis.
|
|
|
|
PiHKAL #106 (MDE): Synthesis of MDE from MDA via N-acetyl-MDA. Synthesis
|
|
of MDE from MDP-2-P using aluminum amalgam. Synthesis of MDE from
|
|
MDP-2-P using sodium cyanoborohydride. The latter two are the most
|
|
useful. Synthesizing MDE from MDA is not particularly useful to
|
|
clandestine chemists.
|
|
|
|
PiHKAL #109 (MDMA): Synthesis of MDMA from MDA via N-formyl-MDA. Synthesis
|
|
of MDP-2-P from isosafrole. Synthesis of MDP-2-P from beta-nitro-
|
|
isosafrole. Synthesis of MDMA from MDP-2-P using aluminum amalgam.
|
|
The synthesis of MDP-2-P from isosafrole and the aluminum amalgam
|
|
synthesis are probably the most useful. The synthesis of MDP-2-P from
|
|
beta-nitroisosafrole might be useful, but most often beta-nitroisosafrole
|
|
is used to produce MDA directly. Synthesizing MDMA from MDA is not
|
|
particularly useful to clandestine chemists.
|
|
|
|
PiHKAL #114 (MDOH): Synthesis of MDOH from MDP-2-P using sodium
|
|
cyanoborohydride. This stuff is active, and the synthesis is useful.
|
|
|
|
Unfortunately, i haven't found an explicit synthesis for MDMA using
|
|
sodium cyanoborohydride. Substituting the correct number of moles of
|
|
methylamine for ethylamine in the MDE synthesis *should* work okay. Also,
|
|
substituting methylamine for ethylamine in the cyanoborohydride synthesis
|
|
produces better yields.
|
|
|
|
NET SOURCES:
|
|
|
|
ftp://ursa-major.spdcc.com/pub/pihkal
|
|
the text of book 2 of PiHKAL with all the syntheses
|
|
http://stein1.u.washington.edu:2012/pharm/pihkal-ht/pihkal.index.html
|
|
html version of PiHKAL
|
|
ftp://hemp.uwec.edu/pub/drugs/psychedelics/mdma/mdma.mda.syntheses
|
|
ftp.hmc.edu:/pub/drugs/mdma/mdma.mda.syntheses.Z
|
|
the synthesis of MDP-2-P from PiHKAL, plus the Leukart reaction from
|
|
Psychedelic Chemistry.
|
|
ftp.hmc.edu:/pub/drugs/mdma/mdma.synth.Z
|
|
this is the safrole + HBr method out of Secrets of Methamphetamine
|
|
Manufacturing
|
|
|
|
ROAD HAZARDS:
|
|
|
|
Chemical Abstracts 52, 11965c (1958): In the synthesis of MDA from MDP-2-P
|
|
this reference has a misprint that should read "add 100ml H2O" instead
|
|
of "add 100ml H2O2" which would cause an explosion. Chemistry is
|
|
dangerous, and a little ignorance can cause spectacular pyrotechnics...
|
|
Psychedelic Chemistry: The synthesis for MDA/MDMA is the same as the
|
|
above Chemical Abstracts reference including the explosive typo. There
|
|
is also another typo which should read "75 ml 15% HCl" instead of "57ml
|
|
15% HCl." This might simply mess your yields up.
|
|
Et20/THF: AKA diethyl ether and tetrahydrofuran. These two chemicals form
|
|
explosive peroxides when they are exposed to air for extended periods of
|
|
time, and which are easily set off by refluxing (for example). These are
|
|
likely the cause of most explosions and fires in amphetamine labs. Do not
|
|
play around with these chemicals, and if you use them, know what you are
|
|
doing.
|
|
MDP-2-P: "piperonylacetone" is an ambiguous term which might refer to the
|
|
4-carbon analogue of MDP-2-P. Shulgin has noted that at least one chemical
|
|
supply house has sold this 4-carbon analogue as "piperonylacetone." The
|
|
correct piperonylacetone (MDP-2-P) is sassafras-smelling oil that is
|
|
yellow colored. The incorrect piperonylacetone has a weak terpene smell
|
|
and is white and crystalline. Substitution will merely result in some
|
|
interesting 4-carbon analogues of MDMA which are probably totally
|
|
inactive. See PiHKAL #109 (MDMA).
|
|
LAH: Lithium Aluminum Hydride (LiAlH4), is a chemical which explodes on
|
|
contact with water, and can be set off by moisture in the air. It should
|
|
only be used under an inert atmosphere, which requires special equipment.
|
|
|
|
--
|
|
Lamont Granquist (lamontg@u.washington.edu)
|
|
"And then the alien anthropologists - Admitted they were still perplexed - But
|
|
on eliminating every other reason - For our sad demise - They logged the only
|
|
explanation left - This species has amused itself to death" -- Roger Waters
|
|
|
|
|