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               Electroreductive stnthesis of mescaline by Dwarfer
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Hi dude... I recently translated J. Prakt. Chemie (1930) electrochemical
reduction of 3,4,5-trimethoxy-betanitrostyrene to mescaline, and will post
it to a.d.c as soon as it becomes practical for me to do so. Some of the
materials (porcellain made to proprietary specifications) are not
available but adequate ceramics almost certainly exist for substitution,
notably sintered borosilicate with a pore size of about 20 microns.

> Good luck

You too.

<predator>

Subj: Electrocatalytic-hydrogenation of nitrostyrenes

This is a posting of a translation from p346 of Journal fur Praktiche
Chemi (Vol 137) from the year 1933. Authors K. H. Slotta and G. Szyszka,
pertaining to the electrolytic reduction of
3,4,5-trimethoxy-beta-nitrostyrene to Mescalin. Probably works on a lot of
Shulgin-type precursors too.

I have yet to scan in the diagram which puts the equipment into some sort
of configurational significance. If it happens that I never get around to
doing that, you have the reference and can probably look it up. The
picture doesn't need translation from German.

ccm = ml ... a cubic centimetre. Letters in brackets refer to parts of the
picture.

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A) Equipment for electrolytic reduction

An anode cell (Z) - a porous cell of Haldenwanger porcellain - was placed
in a filter assembly of 500 ccm (F) volume. The anode had measurements of
75mm x 160mm with a 70mm wide glazed edge that prevented the drawing-up
and smearing of the liquid to be reduced.

To the anode cellwas added a solution of 25ccm concentrated sulfuric acid
in 175ccm water.The anode used was lead or carbon rod and was enclosed in
a tightly wound, glass spiral cooler. The water in this was conducted to
the outer container to help cool the inner tube. By regulating the cooling
water it was possible to keep the whole reduction solutionfor the first
six hours at 20 degrees Celsius. In the last hours the temperature was
allowed to rise to 40 degrees Celsius, to get a nearly quantitative course
of the reduction.

The outer container contained a cathode (K) - a lead sheet (200mm x 90mm x
2mm), which before each experiment was coated electrolytically using
diluted sulfuric acid, with lead superoxide.

B) Reduction

A solution of 30g 3,4,5-trimethoxy-beta-nitrostyrene in 100ccm glacial
acetic acid and 100ccm ethanol was mixed with 50ccm concentrated
hydrochloric acid and added to the cathode container. The anode cell was
filled with dilute sulfuric acid to the outer level of the cathode cell.
Now a current of 5 to 6 amps was passed through the equipment for 12
hours, so that the current density was about 3 amps.

After the finished reduction, the contents of the cathode cell was
filtered and dried under vacuum. The remainder was then dissolved in
300ccm water. Any remaining unchanged nitrostyrene was removed by twice
shaking it out with ethyl acetate. The ester in the solution was then
removed by shaking out once with diethyl ether.

The liquid thus obtained of chloride of mescaline was then put in a
separating funnel which had ether added. The amine was freed with a cold
concentrated solution of technical sodium hydroxide. The solution
obtained, after extracting four times with ether, was dried with calcium
carbonate and the amine precipitated with dry hydrochloric acid gas.

After twice dissolving in absolute, dry, denatured alcohol, completely
pure mescalin hydroxide was obtained as white leaf with a melting point of
184 degrees Celsius and a yield of 24g (77.3%)
