反应详情

In a stream of nitrogen and at 0° C., 0.12 ml (1.30 mmol) of acetic anhydride was added to an anhydrous tetrahydrofuran (10 ml) solution containing 500 mg (1.20 mmol) of 3-(4-chlorobenzyloxy)-N-(2-sulfamoylphenyl)benzamide produced in Reference Example 4 and 293 mg (2.40 mmol) of 4-dimethylaminopyridine, the mixture was stirred at room temperature for 1 hour and then the solvent was evaporated under a reduced pressure. The resulting residue was dissolved in ethyl acetate, washed with water, a potassium hydrgensulfate aqueous solution and saturated brine in that order and dried over anhydrous sodium sulfate, and then the solvent was evaporated under a reduced pressure. The resulting residue was recrystallized from an ethyl acetate-diethyl ether mixed solvent to obtain 290 mg (yield: 52.7%) of the title compound.

1. customthe solvent was evaporated under a reduced pressure
2. dissolutionThe resulting residue was dissolved in ethyl acetate
3. washwashed with water
4. dry with materiala potassium hydrgensulfate aqueous solution and saturated brine in that order and dried over anhydrous sodium sulfate
5. customthe solvent was evaporated under a reduced pressure
6. customThe resulting residue was recrystallized from an ethyl acetate-diethyl ether mixed solvent