Prepn. of trichloroacetyl chloride comprises reacting ethanol with trichloroacetyl chloride to form ethyl trichloroacetate, which is chlorinated to form pentachloroethyl trichloroacetate, which is rearranged into trichloroacetyl chloride (2 mols) at 20-200 degrees C in the presence of a tertiary aliphatic, cyclic, heterocyclic or aromatic amine. The net reaction is a chloroxidation of ethanol. Process gives a prod. of 98% purity.
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