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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.
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