反应详情

温度

75 °C

To a suspension of 6-(4-fluorophenyl)-4-(4-piperidyl)-5-(4-pyridyl)-1H-pyrazolo[3,4-b]pyridine (0.24 g, 0.6 mmol, obtained in example 170) in formic acid (0.64 mL), 35-40% aqueous formaldehyde (0.96 mL) was added. It was heated to 70-80° C. for 24 h. It was allowed to cool and 1 N NaOH was added. It was extracted with CHCl3 and the combined organic phases were dried over Na2SO4 and concentrated to dryness. The crude product obtained was purified by chromatography on silica gel using CHCl3—MeOH—NH3 mixtures of increasing polarity as eluent, to afford 47 mg of the desired compound (yield: 19%).

1. additionwas added
2. temperatureto cool
3. extractionIt was extracted with CHCl3
4. dry with materialthe combined organic phases were dried over Na2SO4
5. concentrationconcentrated to dryness
6. customThe crude product obtained
7. customwas purified by chromatography on silica gel
8. temperatureof increasing polarity as eluent