Yes, Foxy, thank you - but the problem isn't solved this way. The problem is the dirt. It insists on staying together w/the product, no matter in what phase and what form it is - at least, it isn't extracted from an alkaline aqueous medium w/toluene. Not in the least degree. SWIM admits he hasn't given this approach much work though - maybee using smth like ethylacetate would work. He finally managed to make some money recently (money, not honey
) so he'll have some in a coupla days.
Also, that patent you mention is a DMS alkylation, which is, AFASWIMK, a much cleaner rxn. I've seen it bee4 - actually, posted an xtract from it some time ago
- see
Post 240420 (missing)
(Antoncho: "Selective monomethylation of hydroquinone", Chemistry Discourse).
So far, all attempts at rextallization were futile
SWIM made a sat'd solution of the oil in hexane by adding toluene in small portions (it doesn't dissolve in hexane alone at all) and diluted it a coupla more times w/toluene - as the shit oils out. He tried the slowest cooling rate he could manage - in fact, setting his fridge to the lowest cooling rate/wrapping the soln in several wool socks - and w/furious scratching - but, alas, to no avail. Oils out, fuck. He'll give it two more shots, and if that fails, he'll try to dilute it yet more, chill well and try to crush it out w/hexane at low temp, using 'slow diffusion' technique - what do you say?
SWIM's also made an xperiment using HMeSO4 and thoroughly dried MeOH - like, the purpose was to run the rxn totally unhydrous. Interestingly, the black precipitate that initially forms in the rxn, wasn't completely dissolved even after 3h (usually gone in 30 min), and when it did, the rxn was significantly darker than under hydric conditions. He hasn't worked it up yet, but
looks like it ain't an improvement of the method - he'll see yet what the yield will bee, though.
That's it for now,
Antoncho
P.S. I'm terribly glad the Hive is back online
Last 3 days have been a time of sorrow and despair for me and my friends
When i saw the words 'hard disk crash' i was really scared that the Hive archives might bee gone for good or something like that... Happily...
all is well that ends well