08-22-02 03:06
No 347527
chromic,
in the write-up on rhod's site you mentioned that the proportions of solvents reagants etc were lifted from various patents and published methods. Has the DCM:alkene ratio been examined by yourself? As far as i can see with this reaction (having seen George bush perform it under the white house, (it works, absolute no brainer because georgy got 60+% yeild)) the role of the solvent is simply because that's what was done back then and maybe for some temperature control, thus if temperature control wasn't a problem, say a jacketed vessel was used, then the solvent volumes could be reduced significantly or entirely removed, the only problem i perhaps see is if the solubility of the peracetic is increased because of the DCM, but what is more polar, DCM or alkene (say iso), they would appear to be on par in my opinion. The same argument holds for the performic really. At reactions end the thing could be flooded with 5%NaOH, to kill off any residual solubility of the alkene in the acetic/peracetic matrix. i would appreciate your thoughts as i am going to watch the bushster give a 1:5 alkene:DCM trial a whirl would appreciate any input, with a view to trialing a solventless run .
wacka wacka wacka
(Synaptic Self-Mutilator)
08-22-02 04:48
No 347561
Yes, you can go lower with the DCM ratios and still be fine. If you read the references, you'll notice I used the higher of the two DCM ratios. You could easily get away with 1.3L DCM / mol instead of the 1.5L DCM / mol that's in the writeup.
(Hive Addict)
08-23-02 05:45
No 347951
The very first time with the performic was successful using exactly half the amount of DCM. It ran hotter, but yield was exactly as in Baal's experiment, 190g or so from 250g iso.
I'm unsure about the peracetic.
there's a big difference between criticizing your government and criticizing your country