ORGLIST: purification of crude 4'-Bromo-4-Chlorobutyrophenone

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From: paul joshua (pauljoshua_in$##$yahoo.com)
Date: Thu Apr 06 2006 - 09:35:19 EDT

  Dear All,
  Ive been having a problem in final stage purification of my crude product on up-scaling.
  Ive synthesised (Crude) 4'- bromo-4-chlorobutyrophenone by friedel crafts rxn using bromo benzene and 4 chlorobutyryl chloride taking EDC as solvent . After the normal work-up the product 4' Bromo-4-Chlorobutyrophenone distilled at 135 -139 C (0.3 torr) at a lab scale succesfully . But on upscaling,while trying to distill ,the vaccum keeps dropping drastically and we are not able to distll the same.We have tried distilling at 3 different facilities and at all the facilities the same problem was encountered.

    Could somebody help me with suggestions to purify the crude or bettering the procedure.
  Thanks in advance
  Paul

                
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