Acetic Anhydride → N-[2-(3-Cyclohexylmethoxybenzamido)benzenesulfonyl]acetamide

In a stream of nitrogen and at 0° C., 0.11 ml (1.10 mmol) of acetic anhydride was added to an anhydrous tetrahydrofuran (10 ml) solution containing 400 mg (1.00 mmol) of 3-cyclohexylmethoxy-N-(2-sulfamoylphenyl)benzamide produced in Reference Example 7 and 237 mg (1.90 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 purified by a silica gel column chromatography to obtain 430 mg (yield: 96.9%) 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 purified by a silica gel column chromatography

ORD-Eintrag

ord-45ab3ecf62ba49548cc9942a67151224

Quelldatensatz

uspto-grants-2003_04

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06555584B1