Acetic Anhydride → HCID 67024770, compound

Participants

Reaction Conditions

Reaction Steps

0.12 ml of acetic acid anhydride are added dropwise to a mixture of 500 mg of 4-[(3-chloro-4-fluoro-phenyl)amino]-6-({4-[2-(ethoxycarbonyl)-piperazin-1-yl]-1-oxo-2-buten-1-yl}amino)-7-cyclopropylmethoxy-quinazoline and 0.18 ml of triethylamine in 5 ml of methylene chloride at 0° C. The reaction mixture is stirred for one hour at 0° C. followed by one hour at room temperature, washed with water, concentrated sodium chloride solution, dried over magnesium sulfate, and concentrated in vacuo. The crude product is purified by column chromatography on silica gel with ethyl acetate/methanol (98:2 to 95:5). Yield: 291 mg (54% of theory), Melting point: 152-156° C. Mass spectrum (ESI+): m/z=625, 627 [M+H]+

Provenance & Evidence