Well swim is back in the game, hes trying out some new things (new to him). back to the oxone reaction with isosafrole. a major problem that swim, as well as many other bees that do not have vacuum filtiration, have with this reaction is the precipitate that forms when the methanol is added to the oxone solution. weve talked about what salt this may be and that it is (as far as swim knows) not necessary for the reaction.
THE preipitate is a pain in the ass, it traps product and makes a mess. what can we do to sucessful get rid of it and not effect yeilds? well heres this:
Addendum by Psychokitty
Now, lately SWIM has applied your methodology along with a few tricks of SWIM's own. Here are several suggestions (some tried, some not):
Filtering the aqueous Oxone solution (prepared according to your specifications)--both diligently and patiently--in order to remove the clarifier (which is a white soot) so that one can obtain a clear colorless Oxone solution.
Not adding the buffer (i.e., the sodium bicarbonate) ensures that the solution remains acidic throughout. Using methanol as the solvent, this does, according to SWIM, yield the diol instead of the epoxide, just as it does in the original biphasic reaction WITHOUT the methanol. Crude yield was somewhere above 90% and in reference to previous performic reactions, smelled and looked (somewhat reddish, viscous) like the real McCoy (according to SWIM)
Also sugessested is distilling the methanol in out of the solution in order to make the preipitate be soluble again. swim will give this a try tomorow.
Very important!!! today swim thought it would be a good idea to try and filter the oxone solution first. well he did so and as of now has very little yellow in the swiriling mix in the flask. duh, to much bicarb in the solution. when you remove the preipitate adjust the bicarbonate amount as well.
Can we do with out hte bicarb completley? it seems taht its possible, it would make things easier for most new bees because they wont have to worry as much about using to much with there brand of oxone.
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