4-Chlorobenzoyl chloride → HCID 13135950, compound

Participants

Reaction Conditions

Reaction Steps

To a mixture of 13.5 g. (50 mmole) ethyl 4-(piperazin-1-yl)-benzoate hydrochloride and 130 ml. anhydrous pyridine are added, at 5°-10° C., 50 mmole 4-chlorobenzoyl chloride. The temperature is allowed to come to 20° C. and the reaction mixture is subsequently stirred for 6 hours at 40° C. After cooling, it is stirred into 400 ml. ice water, extracted twice with 250 ml. amounts of methylene chloride and the organic phase is dried with anhydrous sodium sulphate and evaporated in a vacuum. The residue is triturated with ligroin and recrystallised from 150 ml. ethanol to give 15.6 g. of the desired product as colourless crystals; m.p. 147°-150° C.

Provenance & Evidence