The Hive > Methods Discourse
o2 is the shit
frost:
KrZ,
did it in a room that the temp was 70f, the glass got very warm, have done it in ice bath but the yields sucked for swinf. how much longer should it go if done in a cooler enviroment, read on the old board the best yield u ever got was in a cold 55f room.so the longer the colder the better. sounds cool to swinf. remember you and os discussing the temp vs o2 absorbtion. love the o2 now, only getting a little whitish forerun before the goodies start flowing over.
thanks for the wisdom,
frost 8) ;)
buchiguy:
I read about this procedure on Rhodium a while ago from Spiceboy. I was wondering if anyone has tried using a paint shaker to get that major agitation that is needed to create oxidation? I was also wondering what would happen if we beefed the pressure up to 100 psi?\
I also do NOT like the benzo/wacker because it uses a relatively hard to get, highly toxic substance, that creates a huge amount of difficult to dispose of waste. I can only get this stuff shipped by ground and it is kind of expensive, although the palladium is the real killer.
psychokitty:
The only two times SWIM has tried this reaction with all reactants in the correct proportions was in the "bad-ass" soda-keg. Both times a yellow oil was obtained that did not aminate and when put through several performic reactions, after dehydration of the intermediate, gave the desired ketone. So, if one is interested in isoalkene, this is a good way to go.
My theory is that SWIMM's use of CuCl2 in this reaction was having a corrosive effect on the surrounding stainless steel. KrZ has never reported this problem, so the only conclusion that I can draw is that he has either been lying all this time about the feasibility of this method (not likely) or his kegs are made of a type of stainless steel (possibly 440) that is absolutely resistant to corrosion.
SWIM is going to give this one another shot, but this time is going to coat inner sides of keg with epoxy paint, which is practically invulnerable to all solvents and reagents that it might be exposed to.
Comments?
--PK
KrZ:
Semtex:
I have to side with the KRZ kid on this one, I was in the thread that he speaks of...
::) ::)
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