Ethyl chloroacetate → HCID 54345847, compound

Participants

Reaction Steps

To a solution of 7-chloro-5-(2-chlorophenyl)-2,4-dioxo-1-neopentyl-2,3,4,5-tetrahydro-1H-1,5-benzodiazepine (0.3 g) and chloroacetic acid ethyl ester (0.11 ml) in dimethylformamide (2 ml) was added sodium hydride (60% oil, 40 mg), and the mixture was stirred for 30 minutes at room temperature. To the reaction mixture were further added sodium hydride (40 mg×3) and chloroacetic acid ethyl ester (0.11 ml), which was stirred for 3 hours. To the mixture was then added acetic acid ethyl ester (50 ml), which was washed with water. The solvent was distilled off, and the residue was purified by means of a silica-gel column chromatography (hexane:acetic acid ethyl ester=4:1 v/v as an eluent) to give 0.25 g of colorless crystals, m.p. 152°-153° C.

Provenance & Evidence