反应详情

To a solution of 4-(4-oxo-1-(4-oxocyclohexyl)-4,5-dihydro-1H-pyrazolo[4,3-c]pyridin-3-yl)benzenesulfonamide (30.0 mg) obtained in Example 173 in THF was added 1.6M phenyllithium butyl ether solution (0.194 mL) at −78° C., and the mixture was stirred overnight at room temperature under nitrogen atmosphere. To the reaction mixture was added 1N hydrochloric acid at 0° C., and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated aqueous sodium hydrogencarbonate solution and saturated brine, dried over anhydrous magnesium sulfate, filtered, and concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (ethyl acetate/methanol) to give the title compound (15.1 mg).

1. extractionthe mixture was extracted with ethyl acetate
2. washThe organic layer was washed with saturated aqueous sodium hydrogencarbonate solution and saturated brine
3. dry with materialdried over anhydrous magnesium sulfate
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure
6. customThe obtained residue was purified by silica gel column chromatography (ethyl acetate/methanol)