News:

Registration doesn't require a real email.
Monero Donation Address: 897ESh4QoJgEytJueBPULziMDfNMToXkGMrvtUCJRo2NQRv2CXACHnmEzeMTkwQhnfcZsAc3ctXp6GsedhMfBv983rn5i84

Main Menu

starting material xtc

Started by bbell, August 29, 2002, 09:36:00 PM

Previous topic - Next topic

0 Members and 1 Guest are viewing this topic.

bbell

From J.of Analytical Toxicology vol.6 p.71-75 (1986).By A.T.Shulgin et al., A soln. of piperonal 15 g. in 80 ml. acetic acid was treated with 15 ml. nitroethane and 7 g. anhydrous ammonium acetate, and heated at 100 degrees for 4 hrs. The addition of a few ml. water followed by cooling yielded 8.0 g. 1-(3,4-methylenedioxyphenyl)-2-nitropropene, m.p.97-98 degrees. Recrystallized from acetic acid. This product was dissolved in boiling acetic acid, and added to a suspension of elemental iron (18.0 g. electrolytic grade) in 100 ml. warm acetic acid. The mixture was heated gently, with frequent swirling, until an exothermic reaction ensued. After the reaction had subsided, one liter of water added, and the mixture clarified by filtration. The filtrate was extracted with 75 ml. methylene chloride three times, the extracts pooled, washed once with 5% sodium hydroxide, and the solvent removed in vacuum. Distillation of the residue yielded 4.6 g. 3,4-methylenedioxyphenylacetone as a colourless oil. b.p. 100-110 degrees at 0.2 mm/mercury.
Chemical supply houses sell inacurate chemicals in place of this compound.

Osmium

> A soln. of piperonal in 80 ml. acetic acid

How much piperonal?

I'm not fat just horizontally disproportionate.

carboxyl

Yield doesn't look that thrilling.

Chemical supply houses sell inacurate chemicals in place of this compound.

Huh? which chemical, piperonal or ketone? They wouldn't sell either to me anyway :(

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

Rhodium

Osmium: 15g Piperonal, apparently, even if the above poster doesn't express himself so clearly. This synthesis is very similar to the one in Pihkal #100 for the same nitrostyrene, with the exception of the latter one using cyclohexylamine for a yield of 10.7g, instead of this with NH4OAc, yielding 9g.

Carboxyl: The Shulgin article above discusses the ambiguity of the name "piperonylacetone", which can both mean the three-carbon side-chain compound MDP2P and the four-carbon side-chain homolog (the benzylacetone). This is also discussed in Pihkal, see the extensions and commentary part in

http://www.erowid.org/library/books_online/pihkal/pihkal109.shtml

for details.

bbell

Starting material is word for word from Journal of Analytical Toxicology

carboxyl

Thanks for the clarification, it makes sense now.  :)

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