反应详情

A 220 mg portion of 2-chloro-5-nitrobenzoyl chloride was added to a pyridine solution (10 ml) of 318 mg of 4-{[2-(pyridin-3-yl)piperidin-1-yl]sulfonyl}aniline and stirred overnight at room temperature. After stirring at 50° C. for 4 hours, 220 mg of 2-chloro-5-nitrobenzoyl chloride was further added thereto and stirred at 50° C. for 2 hours. Ethyl acetate and water were added thereto to carry out layer separation operation, and the organic layer was washed with saturated sodium chloride aqueous solution. After drying with anhydrous sodium sulfate, this was concentrated under a reduced pressure and the thus obtained residue was purified by a silica gel column chromatography using chloroform:methanol (98:2) as the elution solvent, thereby obtaining 426 mg of 2-chloro-5-nitro-N-(4-{[2-(pyridin-3-yl)piperidin-1-yl]sulfonyl}phenyl)benzamide as colorless crystals.

1. stirringAfter stirring at 50° C. for 4 hours
2. stirringstirred at 50° C. for 2 hours
3. customlayer separation operation
4. washthe organic layer was washed with saturated sodium chloride aqueous solution
5. dry with materialAfter drying with anhydrous sodium sulfate
6. concentrationthis was concentrated under a reduced pressure
7. customthe thus obtained residue was purified by a silica gel column chromatography