反应详情

A solution of 2-amino-5-pyrazin-2-yl-4-trifluoromethyl-benzoic acid methyl ester (235 mg, 0.79 mmol) and 4-chlorophenyl chloroformate (133 μL, 0.95 mmol) in dioxane (8 mL) was stirred at 80° C. for 105 min. After cooling to r.t., CH3SO2NHNH2 (130.6 mg, 1.19 mmol) and i-Pr2NEt (276 μL, 1.58 mmol) were added. The mixture was heated to 80° C. for 45 min, cooled to r.t., and the solvent was removed in vacuo. The residue was purified by flash chromatography (50 g silica gel, DCM→MeOH in DCM (2% to 5%)) to provide the title compound (241.5 mg, 76%) as a white powder. API-ES: m/z 402 [M+H]+, rt 2.69 min.

1. temperatureThe mixture was heated to 80° C. for 45 min
2. temperaturecooled to r.t.
3. customthe solvent was removed in vacuo
4. customThe residue was purified by flash chromatography (50 g silica gel, DCM→MeOH in DCM (2% to 5%))