chemrox - 4-2-2013 at 12:45
Is 14 mm ST semi-micro? Anyway I'm moving toward the 1 mmol from the 10 mmol experimentation level. I have a lot small flasks and a good partial
takeoff vacuum still head. I don't have a column, condenser or simple still head. Another issue is workup. At the 1 mmol level I think
chromatography is going to work a lot better than distillation and recrystallization. Maybe I need one of those "baggy pants" Hickman condensers for
simple distillation. But a smaller flash chromatography setup would seem a must. This could become rather expensive in terms of stationary phase
replacement. Or running lots of solvent through to clear out residual tars and the like. Comments? Advice?
Thanks!
Chromatotron
radagast - 4-2-2013 at 21:17
How about using a Chromatotron or Cyclograph to purify ~100 mg. to 1 gram of product? I've played around with one and you rarely need more than a few
hundred mls of solvent, and you can reuse (and easily make) silica or alumina plates.