posted 02-05-2000 12:49 AM         

•Gently reflux for 5-6 hours
•Cool and distill off any residual nitromethane.
-If the crystaline mass prevents distillation, remove it by vacuum filtration and use what is collected OR distill off the filtered nitromethane solution to collect an additional crop of crystals (If the crystals are stuck in the flask skip to the next step)
•Add enough boiling MeOH to dissolve the entire mass (If it's stuck in the flask, if not skip this step, filter, and recrystalize once from boiling MeOH)
•Decant, cool and vacuum filter, repeat the recrystalization if the crystals are not a pure yellow color (which they usually are)

Hydrogenation;
15g Pd/C 5%
175g 3,4,5TMBnitrostyrene
2.5L Anhydrous EtOH
100ml 31.45% HCl
•Add reagents to the keg, begin vigorous stirring
•Remove atmosphere and pressurize to 75psi with H2
•React for 8-10 hours or until H2 uptake has completely ceased
•Evacuate H2 outside, vacuum out interior of vessel, allow H2 to clear, THEN open the vessel
•Vacuum filter off Pd/C
•Re-filter through celite for maximum Pd/C recovery/removal
•Distill the mixture down until the Ethanol fraction begins to cease
•Cool and take up what is left in 2L 3N HCl
-Your remainder may look somewhat black/brown here, but don't worry, this will all be cleared up. If the hydrogenation did not go to completion some unreacted nitrostyrene will remain, this should be filtered from the solution.
•Wash with 2x125ml DCM
•Basify to pH>11 dropwise and with stirring with saturated NaOH solution
•Extract 3x125ml DCM
•Dry over NaSO4 (250g) for 15 minutes
•Filter off NaSO4 and bubble DCM with HCl(g) anhydrous. After crystalization ceases it can be advantageous to filter and redry the DCM with another 100g NaSO4, then bubble some more.
•Collect HCl salt crystals by filtration

Final mass yield = 168.74g M•HCl

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posted 02-05-2000 05:36 PM         

The styrene isn't too much of a problem. But the reduction is somewhat
uncool.

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.

--psyloxy--

posted 02-07-2000 12:00 AM         

i meant regarding 2c-b, dom, etc.: "And have fun trying to get it to work, I've had major snags trying to run similar reactions."

posted 02-08-2000 05:00 PM         

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This post contains information for educational purposes only. Anyone under the age of 18 must not read this post and must leave NOW. This post contains information about certain chemicals that are illegal to posess, manufacture, and distribute. Any person caught breaking the law is subject to prosecution to the fullest extent of the law. This post also contains information for manufacturing hazardous, posionous, and explosive chemicals. These are only intended for those who have experience, applicable licenses for and the equipment to do so. Any accident is not the responsibility of this poster.