Ammonia → HCID 67024573, compound

Participants

Reaction Steps

1 ml of ice-cooled concentrated hydrochloric acid is added to 340 mg of 4-[(3-bromophenyl)amino]-6-((4-[N,N-bis(2,2-diethyoxyethyl)amino]-1-oxo-2-buten-1-yl)amino)-7-methoxy-quinazoline while cooling with an ice bath. The mixture is left to stand for 3 hours before 1.5 ml of concentrated ammonia solution is added dropwise while cooling with an ice bath for working up. The precipitate formed is suction filtered and washed with water. The crude product is purified by chromatography on a silica gel column with methylene chloride/methanol (20:1) Yield: 50 mg (17% of theory) Melting point: 133-138° C. Mass spectrum (EI): m/z=585, 587 [M]+

Provenance & Evidence