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- Chem Dweebs, how does this look?
-
- MDA (3,4-methylenedioxyamphetamine)
-
- The following synthesis is not meant to be carried out by a novice
- chemist, although it is not terribly difficult. For descriptions of
- how to carry out the procedures, a standard lab procedures reference
- manual should be aquired by the reader (or preferably the reader
- should take college organic chemistry).
- This is the synthesis for MDA which can be found on page 79 of
- Psychedelic Chemistry, which was first published in Chemical Abstracts
- 52, 11965c (1958). The former however has the above noted
- typographical error of 75 ml 15% HCl being written as 57ml 15% HCl.
- The original article also has a typographical error. In the synthesis
- of MDA from the ketone it reads H2O2 where it should read H2O --
- following the former procedure would be explosive. As a side note,
- this is the same process of making the ketone from isosafrole as
- Shulgin uses in PiHKAL, thus the synthesis of the ketone is somewhat
- more verbose than the synthesis of MDA from the ketone.
-
- To a well stirred, cooled mixture of 34g of 30% H202 (hydrogen
- peroxide) in 150g 80% HCO2H (formic acid) there was added, dropwise, a
- solution of 32.4g isosafrole in 120ml acetone at a rate that kept the
- reaction mixture from exceeding 40 deg C. This required a bit over
- 1 hour, and external cooling was used as necessary. Stirring was
- continued for 16 hours, and care was taken that the slow exothermic
- reaction did not cause excess heating. An external bath with running
- water worked well. During this time the solution progressed from an
- orange color to a deep red. All volatile components were removed under
- vacuum which yielded some 60g of a very deep residue. This was
- dissolved in 60ml of MeOH (methyl alcohol -- methanol), treated with
- 360ml of 15% H2SO4 (sulfuric acid), and heated for 3 hours on the
- steam bath. After cooling the mixture was extracted with 3x75ml
- Et2O (diethyl ether) or C6H6 (benzene). Its recommended that, the
- pooled extracts can washed -- first with H2O and then with dilute NaOH
- (sodium hydroxide). Then the solvent is removed under vacuum to
- afford 20.6g 3,4-methylenedioxyphenylacetone (3,4-methylenedioxybenzyl
- methyl ketone). The final residue may be distilled at 2.0mm/108-112 deg
- C, or at about 160 deg C at the water pump.
- Add 23g 3,4-methylenedioxyphenylacetone to 65g HCONH2 (formamide)
- and heat at 190 deg for five hours. Cool, add 100ml H20, extract with
- C6H6 (benzene) and evaporate in vacuum the extract. Add 8ml MeOH
- (methyl alcohol -- methanol) and 75ml 15% HCl to residue, heat on
- water bath two hours and extract in vacuum (or basify with KOH and
- extract the oil with benzene and dry, evaporate in vacuum) to get
- 11.7 g 3,4-methylenedioxyamphetamine (MDA).
-
- To produce MDMA substitute N-methylformamide for formamide in the
- above synthesis.
-
- Comments?
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