The Hive > Novel Discourse
New method for P2P
bio:
OK, the procedure done per the Berliner article (as much as could be deciphered anyway), details above, sat 39 hrs at ambient (ca 20deg). Washed with NaOH separated all but the last few drops to let settle a while. When ready to do the water wash noticed the crystals had already set up in the funnel. Heating the funnel now to melt the stuff. This has never happened before, hopefully a portend of the greater yield.
Bwiti:
"There is a French reference somewhere that states that the condensation can be done by reluxing equal volume amounts of benzaldehyde and butanone with hydrochloric acid and there are also references using H2SO4. I have tried both of these and did not get the result that I did using dry HCl gas."
Perhaps anhydrous HBr gas could be used instead? Dry HBr is easier for me to make.
hoffman:
You would think that oxone(Potassium Peroxymonosulfate) might bee good here for the per-acid.
2 cents,
This is a reaction deserves another look,!
hoff
Megatherium:
You would think that oxone(Potassium Peroxymonosulfate) might bee good here for the per-acid.
2 cents,
This is a reaction deserves another look,!
Toluene can be oxidized to benzaldehyde with persulphate:
Post 208719 (Osmium: "Re: The easiest synth of benzaldehyde from toluene", Chemistry Discourse)
Condense the prepared benzaldehyde with MEK and do the Baeyer-Villiger with K2S2O8 - H2SO4 (ref.: Billups, Kramer, Lastomirsky: J. Org. Chem. (1970) vol 35, p 3080)
Hydrolize et voilà.
Megatherium:
I have only access to the first page of this article online ::)
The abstract says:
'Solutions of K2S2O8 in 20 - 60 % H2SO4 are advantageous for the Baeyer - Villiger oxidation of ketones. Yields are quantitative and the differences in migratory aptitudes are larger than those found with other peracids.'
I guess the enol ester just will rearrange in situ to the P2P in the acidic environment (1 pot).
Now, I have been informed that somebee wants to try out this reaction. Unfortunately, I can't get the journal in my hands until next month.
It would really surprise me if there was nobee with online access to the full journal. I 'm sure the involved bee will produce a nice write-up for the hive collective.
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