bbell
(Stranger)
08-29-02 21:36
No 350445
       starting material xtc
(Rated as: excellent) 		 Bookmark   

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
(Stoni's sexual toy)
08-29-02 22:11
No 350452
       > A soln. of piperonal in 80 ml.  Bookmark   

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

How much piperonal?
I'm not fat just horizontally disproportionate. 		 
 
 
 
    carboxyl
(Hive Bee)
08-30-02 05:30
No 350588
       Yield doesn't look that thrilling.  Bookmark   

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 anywayfrown
The above post is purely fictional. Any resemblance to "real-life" is purely coincidental. 		 
 
 
 
    Rhodium
(Chief Bee)
09-02-02 17:40
No 351822
       Piperonal & Piperonyl  Bookmark   

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
(Stranger)
09-02-02 20:59
No 351881
       post is true  Bookmark   

Starting material is word for word from Journal of Analytical Toxicology 		 
 
 
 
    carboxyl
(Hive Bee)
09-03-02 09:35
No 352181
       can see clearly now  Bookmark   

Thanks for the clarification, it makes sense now. smile
The above post is purely fictional. Any resemblance to "real-life" is purely coincidental.