Hexanoyl chloride → N-[2-[3-(4-Methoxybenzyloxy)benzamido]benzenesulfonyl]hexanamide

In a stream of nitrogen and at 0° C., 0.15 ml (1.10 mmol) of hexanoyl chloride was added to an anhydrous tetrahydrofuran (10 ml) solution containing 400 mg (1.00 mmol) of 3-(4-methoxybenzyloxy)-N-(2-sulfamoylphenyl)benzamide produced in Reference Example 6 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 490 mg (yield: 98.8%) 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-52510eeda4c8443e9b5215e114de0c5d

Quelldatensatz

uspto-grants-2003_04

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06555584B1