反应详情

In a volumetric flask, 2-[4,6-bis(4-fluorophenyl)-5-(4-pyridyl)pyrazolo[3,4-b]pyridin-2-yl]acetaldehyde (0.08 g, 0.2 mmol, obtained in example 94), sodium triacetoxyborohydride (0.08 g, 0.4 mmol), 4-hydroxypiperidine (0.02 g, 0.2 mmol) and 1,2-dichloroethane (3 mL) were introduced under argon atmosphere. The mixture was stirred overnight at room temperature. It was concentrated and a mixture of water and EtOAc were added. The phases were separated. The aqueous phase was extracted with EtOAc. The organic phase was dried over Na2SO4 and concentrated to dryness. The crude product obtained was purified by chromatography on silica gel using increasing polarity mixtures of EtOAc-MeOH as eluent, to afford 19 mg of the title compound (yield: 20%).

1. concentrationIt was concentrated
2. additiona mixture of water and EtOAc
3. additionwere added
4. customThe phases were separated
5. extractionThe aqueous phase was extracted with EtOAc
6. dry with materialThe organic phase was dried over Na2SO4
7. concentrationconcentrated to dryness
8. customThe crude product obtained
9. customwas purified by chromatography on silica gel using
10. temperatureincreasing polarity mixtures of EtOAc-MeOH as eluent