Author Topic: synthesis xtc  (Read 1193 times)

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bbell

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synthesis xtc
« on: September 02, 2002, 09:39:00 PM »
From:Journal of Pharmaceutical Sciences vol.69(10)p.192-5(1980)by Ulrich Braun et.al.
To a soln. of 25 g. methylamine hydrochloride in 110 ml. methanol were added 6.6 g. of piperonylacetone and then 3.0 g. sodium cynoborohydride. The mixture was stirred at room temp., and concentrated hydrochloric acid was added as required to maintain the pH to neutrality. The reaction was copmplete in 36 hours. Following addition to one liter water containing 5 ml. of conc. HCL, the reaction mixture was extracted twice with 150 ml. of methylene chloride (discarded), made basic with 25% sodium hydroxide, and reextracted with 3 X 150 ml. of methylene chloride. The extracts were pooled, and the solvent removed in vacuum.
  Distillation of the residue oil (8.4 g.) at 0.40 mm mercury yielded 6.1 g. of product as a viscous oil, b.p. 100-110 degrees. This product was dissolved in 60 ml. of isopropanol and acidified with conc. HCL (titration end point determined with external damp universal pH paper), and an equal volumn of ether was added. There was a spontaneous crystallization of the product as a white solid. It was removed by filtration and washed first with isopropanol-ether and finally with ether alone, giving 6.2 g. of the air-dried product (74% yield), m.p.151-152 degrees.
This post is word for word from said journal

carboxyl

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cool
« Reply #1 on: September 03, 2002, 09:46:00 AM »
another reference to add to the sack. This "professional" production of MDMA uses titration rather than gassing for final crystalline product recovery. I am assuming that these people, Ulrich Braun et.al., are going to be using the most effecient and highest yielding steps to the product. Is there an actual advantage to titrating, than gassing. Safety is obviously a factor. So why didn't these guys gas, if gassing is considered better by some?

ps. To a soln. of 25 g. methylamine hydrochloride in 110 ml. methanol were added 6.6 g. of piperonylacetone

hopefully they used the right kind of "piperonylacetone"  ;)

The above post is purely fictional. Any resemblance to "real-life" is purely coincidental.

Osmium

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> This "professional" production of MDMA uses ...
« Reply #2 on: September 07, 2002, 11:18:00 PM »
> This "professional" production of MDMA uses titration
> rather than gassing for final crystalline product
> recovery. I am assuming that these people, Ulrich Braun
> et.al.,

I could be wrong, but I think that Braun guy has co-authored at least one paper with Shulgin.

> are going to be using the most effecient and highest
> yielding steps to the product.

No. They use procedures that are known to work, are easy to perform, are known to the researcher and which the researcher likes best for purely personal reasons (often some weird, unsubstantiated preference).

> Is there an actual advantage to titrating, than gassing.
> So why didn't these guys gas, if gassing is considered
> better by some?

It easily produces a clean sample of the desired amine hydrochloride, but not a super high yield!

I'm not fat just horizontally disproportionate.