Drying high-melting cpds - contg high-boiling org solvent by heating with water

摘要

High-melting cpds are dried by (a) prepg. a mixt of water and a solid halogenated org. cpd. (I), which is moist with a water-immiscible org. solvent (II) with b.pt. >145 degrees C; (b) heating the mixt. to remove (II) and (part of) the water; and (c) drying the aq. (I) mixt. freed from (II) to give dry, free-running (I) particles. (I) pref. is halogenated (brominated) adduct of styrene and a halo(hexachloro-)cyclopentadiene or tetrabromo-2-chlorotoluene, (II) has b.pt within 30 degrees C of the m.pt of (I) and pref. is C2HCl5, CHBr3 and/or esp. CHCl2.CHCl2. Heating is carried out at reduced press.