反应详情

温度

60 °C

To a solution of 4,6-bis(4-fluorophenyl)-5-(4-pyridyl)-1H-pyrazolo[3,4-b]pyridine (0.20 g, 0.5 mmol, obtained in example 1) in DMF (5 mL), N-chlorosuccinimide (0.10 g, 0.8 mmol) was added under argon atmosphere and the mixture was heated to 60° C. for 5 h. It was washed with 1 N NaOH and extracted with CHCl3 and 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 171 mg of title compound (yield: 79%).

1. washIt was washed with 1 N NaOH
2. extractionextracted with CHCl3 and EtOAc
3. dry with materialThe combined organic phases were dried over Na2SO4
4. concentrationconcentrated to dryness
5. customThe crude product obtained
6. customwas purified by chromatography on silica gel
7. temperatureof increasing polarity as eluent