1,1,1,2-Tetrachloroethane → HCID 13154195, compound

Participants

Reaction Steps

Aluminum chloride (231 mg.) was added all at once to a mixture of 160 mg. of 4-cyano-N-(1,2-dichloro-2-phenylethyl)pyrrole-2-carbonyl chloride and 0.5 ml. of tetrachloroethane controlled at 140° C. After 4-5 minutes, the mixture is cooled, 15 ml. of water is added and the mixture is extracted with 4 × 10 ml. of chloroform. The extract is washed with water, dried and chromatographed on 10 g. of silica gel by elution with benzene:ethyl acetate (3:1 v/v). The first fraction provided 47 mg. (33%) of 2-cyano-5,6-dichloro-6,11-dihydro-5H-[2,1-b][3]benzazapin-11-one, m.p. 213°-223° C.

Provenance & Evidence