posted 02-05-2000 07:16 PM         

Till now i've copy-paste'ed the following notes:

5g of piperonal, 5ml of nitroethane ans 2g of ammonium acetate are added to 20 ml of glacial acetic acid. The resulting solution is refluxed for two hours and then poured into ice-water. The solution is cooled in an ice-bath overnight and the crystals filtered out and allowed to dry.

-- this is from tcboe as you can see, but I think it would not be
-- problematic to substitute the aldehyde (as long as molar ratios
-- are the same)

For the reduction I think I'll go deeper into the electrochemical
one.

Again here's something from the complete book of ecstacy:

Although I have seen many references to the use of electrochemical cells, the construction of them I have yet to see thoroughly described or for that matter where they can be purchased. This doesn't mean they are impractical, because for clandestine chemistry where the most reliable reduction reagents are watched like a hawk, electrochemical reductions could be the next breakthrough.

The cells are basically a container divided by some material which will allow charged ions to pass and therefore allow electricity to flow. The membrane also halts the flow (or reduces it considerably) of the material being reduced. This is necessary because if the membrane wasn't there, the reduced product could travel to the other electrode and become oxidized. The membranes are made of such materials as sintered glass, cellophane, porous ceramic plates etc.

This procedure was written for the analogous nitrostyrene which would lead to amphetamine. It should work equally well for MDA[46].

207g (1 mole) of the nitrostyrene is dissolved with a solvent prepared by mixing one liter of ethanol with 500ml of acetic acid and 500ml of 12N sulfuric acid. The solution is placed in the cathode compartment of a divided electrolytic cell containing a mercury, copper or metal of similar nature as the cathode electrode. The anode can be made of lead. 3N sulfuric acid is placed in the anode compartment. Current is passed equaling ~0.2 amperes/cm2 of cathode surface. The temperature is kept between 30-40°C during the electrolysis until at least 8 Faradays of electricity have passed through the solution.

The number of square centimeters of your cathode surface (count both sides if both sides are in contact with the solution) times 0.2 is the amount of current you need flowing through your cell. 1 Faraday is equal to 96485.309 coulombs/mole of electrons and 1 Ampere is equal to 1 coulomb/second. The amount of time in hours the reaction should be run is then 771882.5 divided by the number of Amperes divided by 3600. If you have a total cathode electrode area of 40 cm2 then you need 8 Amperes running through your cell for 26.8 hours.

Remove the ethanol and ethyl acetate present through distillation (quit distilling when the temperature approaches 100°C). Basify the remaining solution with 25% NaOH and extract the MDA from the solution with 3 portions of ether (or toluene or methylene chloride). Wash the extract with several portions of calcium carbonate solution, water and then dry with magnesium sulfate. Filter out the drying agent. Pass HCl gas through the solution until no more precipitate is formed. Filter the crystals and wash with ether and allow to dry.
(Still searching for a xtalization that doesn't use HCl gas...)

I think all in all this is really easy and safe.
You don't need a vacuum. The chems are not too toxic and
readily available (if u know where to look).
You don't have to boil EtO2 for 24h etc...

So anybees out there who want to make this work ?
I think the reduction still needs further investigation.
But I would be happy to hear if someone told me that he
successfully dreamt this.

One main question seems to be where one gets the electrolysis
cell from. Well, SA has electro-equipment. But I don't understand
anything if I see no picture. Would also be nice to know how one
manages the current (transformer or what ??).

C'mon people this is not only useful for M but also 2C-H and 25DMA, the
precoursers to lovely substances like 2C-B, 2C-C, DOB and DOC.

Uhhm in some older topic KrZ said he tried a way like this with 'major snags'. Which were them ?

posted 02-06-2000 09:39 AM         

This was posted to the Hive by dwarfer [06-24-99 05:04 PM]:

[dwarfer]

With regards to my on line correspondent, Predator, with whom I was discussing my usual pressurized dreams:
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.

--------------------------------------------------------------------------
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%)

--------------------------------------------------------------------------
<predator>

[/dwarfer]

Well, I'd definitely like to see the picture and the original
german article as well.

Nobody seems to know from what they should build an
electrlysis cell. But like I said: SA sells some
equipment. And since I now know that the hoffman app is
yes- the most expensive but no- not usable (2 H2O -> 2H2 + O2).

Then the question is: whats a Brownlee apparatus ?

Fuck it. That looks really easy. Look at these chems: GAA, H2SO4, HCl, EtOH, NaOH... sounds much better then LAH in Et2O for me. Especially much more OTC.

So why not discuss it ?! This is the future !
There must be some electrochemists out there!
(yeah Rhodium I know this is not you )

posted 02-06-2000 01:52 PM         

You could just grow it you know.
Try erowids vaults and cactus.

posted 02-06-2000 02:11 PM         

dont flame me !

posted 02-06-2000 06:50 PM         

This nitroethane is there 'cause it is taken from the complete book of xtc.
There they want to make an amphetamine (MDA) and so logically they use EtNo2.

But my intention in posting this was only to show that there was an easy method for general use to get the nitroAlkene.
(In fact they are all very easy but this one I liked best)

much said. nothing new.

So on with the show:

this is from WizX' Xf-3 'ELECTROCHEMICAL REDUCTION OF NITROPROPENYLBENZENE '
NITROPROPENYLBENZENE

Nitropropenylbenzene is another name for phenylnitroproene, which is one CH3- longer then Nitrostyrene (or phenylnitroethene) I assume.

"The current is kept at 3.5 Amps for 3 hours (10800 C), then 4.5 Amps for 2 hours (7200 C), then 5.0 Amps for 5 hours (18000 C), a total of 10 hours and 160,200 Coulombs of electrons"

Is this neccesary ? Or just to get the rxn done fast ?

I had a look at my electronics catalog and
they have power supplies with 2/4/6/8/12 amp
and all 13,8V. Do I need an ammeter ?

In this file a clay pot is used.
Would be intresting if it has been dream-tried. Fester saiz it works. Rhodium doubted it. For me it would be intresting where to get something that surely works (and for that matter what a Brownlee apparatus is(which is sold by the SA))

SA also has all sorts of electrodes but not Pb. Which one to use instead ? Copper and carbon where mentioned.