Originally posted by Mendeleev
Chloroacetone [1]
Good method of preperation 150 ml acetone 50 ml water 12 g Cupric chloride 6 g lithium chloride. Reflux till reaction completes. Literature states 24
hours but the reaction has a half-life of about 24 minutes at 20°C (same article half of marker in 24 minutes, the marker being oxygen consumption in
a slightly different reaction), therefore 5 hours is probably sufficient at reflux.
After reacting, distill everything below 123°C. The still bottoms can be reprocessed to recover cuprous chloride and lithium chloride. Both can be
recovered by disolving with minimum water. The mix is easily converted to cupric chloride-lithium chloride by boiling with 20-35% hydrochloric acid.
Redistill slowly through a packed column to remove acetone. This leaves two fractions one distilling at 89C which is water and chloroacetone and the
second distilling at 121°C which is ?pure? chloroacetone. The second fraction may contain unsymetrical dichloroacetone I haven't had a sample
analysed. Calcium Chloride will crash the water-chloroacetone mix which tends to form a colloidal solution.
Chloroacetone must be stabalized with 1% calcium carbonate or 0.1% water if it is stored or it forms an explosive sludge. Distillation of a
water-chloroacetone mix at 89°C is the most efficient way of separating unsym-dichloroacetone from commercial products.
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