反应详情

A solution of KOH (0.07 g, 1.3 mmol) in tBuOH (2.5 mL) was added under argon atmosphere to 4,6-bis(4-fluorophenyl)-5-(4-pyridyl)-1H-pyrazolo[3,4-b]pyridine-3-carbonitrile (0.05 g, 0.1 mmol, obtained in example 65) and heated to reflux overnight. Water and EtOAc were added and the phases were separated. The aqueous phase was extracted with EtOAc. The combined organic phases were dried over Na2SO4 and concentrated to dryness. The crude product obtained was purified by chromatography on silica gel using hexane-EtOAc mixtures of increasing polarity as eluent, to afford 15 mg of the title compound in solid form (yield: 28%)

1. temperatureheated
2. temperatureto reflux overnight
3. customthe phases were separated
4. extractionThe aqueous phase was extracted with EtOAc
5. dry with materialThe combined organic phases were dried over Na2SO4
6. concentrationconcentrated to dryness
7. customThe crude product obtained
8. customwas purified by chromatography on silica gel
9. temperatureof increasing polarity as eluent