wacko_reaco (Hive Bee)
06-14-02 05:49
No 321036
      scale-up limitations for oxone route to epoxide  Bookmark   

Hello all,
Just wanting to start a discussion on the factors a(e)ffecting the scale-up of the oxone reaction. Some-one i know is intending a scaled up trial in a week using a 120L vessel and overhead stirring and thought i would consult my wise hive friends for any insightful advice for them. the results of the trial once posted should prove to help any-one else intersted in this area. This friend of mine has performed scaled up performics to 6kg iso but likes the idea of not needing20L of DCM. Obviously this amount (6kg iso) is not feasible via the oxone route in a 120L vessel but hey as Osmium always says, time is cheap.
Anyhows let the talk fest begin, anyone scaled up anyways?
caio for now

wacka wacka wacka
(Hive Addict)
06-14-02 22:01
No 321351
      Oxone  Bookmark   

Stirring is crucial to the rxn.use a propellar or something.  Watch the heat.  If it goes over 40 your screwed.  Make sure your vessel is elevated off the ground and has a drain in the bottom. let the sediment settel and siphoj off the water layer in to the dcm.  set the barrel up like a buchner funneland wash the crystals with EtOH draining it out the bottom into the dcm.