Triethylamine → HCID 54041039, compound

Participants

Reaction Conditions

Reaction Steps

A stirred mixture of 500 mg 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 0.20 ml triethylamine in 5 ml of methylene chloride is cooled in an ice/water bath, and 80 μl of methanesulfonyl chloride are added dropwise. The reaction mixture is stirred for one hour at 0° C. and another two hours at room temperature. Aqueous work-up followed by column chromatography on silica gel with methylene chloride/methanol (97:2) gives the title compound as a slightly yellow solid. Yield: 395 mg (70% of theory), Melting point: 170-173° C. Mass spectrum (ESI+): m/z=661, 663 [M+H]+

Provenance & Evidence