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