反应详情

Potassium carbonate (0.87 g) and 4-phenylsulfonylbutyl chloride (0.40 g) were added to a solution (15 ml) of 4-amino-5-chloro-2-methoxy-N-(piperidin-4-ylmethyl)benzamide dihydrochloride (0.52 g) in dimethylformamide, and the mixture was stirred at 70°-80° C. for 7.5 hr. Water was added to the reaction mixture, and the mixture was extracted with chloroform. The organic layer was washed with brine and dried. The solvent was evaporated under reduced pressure, and the obtained residue was purified by silica gel column chromatography. The obtained oil was treated with hydrochloric acid-ethanol and the obtained crystals were recrystallized from ethyl acetate to give 0.10 g of 4-amino-5-chloro-2-methoxy-N-((1-(4-phenylsulfonylbutyl)piperidin-4-yl)methyl)benzamide hydrochloride.

1. extractionthe mixture was extracted with chloroform
2. washThe organic layer was washed with brine
3. customdried
4. customThe solvent was evaporated under reduced pressure
5. customthe obtained residue was purified by silica gel column chromatography
6. additionThe obtained oil was treated with hydrochloric acid-ethanol
7. customthe obtained crystals were recrystallized from ethyl acetate