The Vespiary
The Hive => Chemistry Discourse => Topic started by: Grignard on January 22, 2004, 06:59:00 PM
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Hello.. I do some experiments on reduction of pn2p by the use of Zinc activated with a temperature of 140-150 degred Celcius for 3 hr under N2 athmosphere... This compound shold take hard on a double bound and since Fe could be used to reduce pn2p to ketone maybe this activated Zn could do the same?? Has Anyone out there tryed this? I have done it but im not shure about the results, the reaction was wery exotermic and the solution turned red and thick and gasses of nitrogenoxide.... :-[ ... Is the p2p soluble in acetic acid??
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woow... this shit realy worked... i dumped the residu from the rxn in vater and ekstract with toluene.. This was washed with 10% NaOH and the tolune was destilled off in vacue... The residual red oily stuff was steam destilled!! and guess what.. ;D light yellow oil of p2p.. I will do this more scientific later, with weight measures etc...
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Zn reduced 4-methoxyphenyl-2-nitropropene to the corresponding ketone (major) and amphetamine (minor). UTFSE for more clues.
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Activated Zn + Cu. Galvani activated !
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The activation procedure is tedious and cumbersome. The zinc-copper couple is labile toward oxygen so it can be stored only for a limited time when reproducible results are to be achieved. Commercicially available zinc can be activated without the need of copper, similar philosophy can be used for the activation of magnesium for the grignard reaction[1]. Bench top zinc powder are heated to 140-150 C with vigorous stirring for a minimum of 3 hours under an inert atmosphere (N2), this is sufficient to activate it. Neither prolonged heating (overnight) nor higher temperatures (170-180) improved the yields or the rate of the reaction significantly.
[1] Baker, K.V., Brown, J. M., Huges, N., Skarnulis, A. J. and Sexton, A., J. Org. Chem. 1991, 56, 698.
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Stirring Zn in 2M HCl for some min. then filtering the Zn off will do the trick as well.