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From: lamont@hyperreal.com (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://www.hyperreal.com/~lamont/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 (lamont@hyperreal.com) "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