反应详情

250 ml of dichloromethane is combined with 9.38 g (52.37 mmol) of 4-fluoro-2-trifluoromethylaniline and 6 ml (14.3 mmol) of pyridine. The mixture is cooled with ice water and under agitation and exclusion of moisture, 13.52 g (57.62 mmol) of 2-chlorosulfonylbenzoic acid methyl ester is added in small increments. The mixture is agitated overnight, washed with 2N hydrochloric acid and water, the dichloromethane solution is dried over sodium sulfate and concentrated to dryness under vacuum. The residue is crystallized from ethyl acetate/hexane. The title compound melts at 143°-145° C.

1. additionis added in small increments
2. washwashed with 2N hydrochloric acid and water
3. dry with materialthe dichloromethane solution is dried over sodium sulfate
4. concentrationconcentrated to dryness under vacuum
5. customThe residue is crystallized from ethyl acetate/hexane