反应详情

To a solution of 4-(6-chloropyridin-3-yl)-6-(4-fluorophenyl)-2-methyl-5-(4-pyridyl)pyrazolo[3,4-b]pyridine (74 mg, 0.2 mmol, obtained in example 193) in AcOH (1 mL), Zn (72 mg, 1.1 mmol) was added under argon atmosphere and the mixture was heated to reflux overnight. It was allowed to cool and concentrated. The residue was treated with saturated NaHCO3 and it was extracted with CHCl3. The organic phase was dried over Na2SO4 and concentrated to dryness. The crude product obtained was purified by chromatography on silica gel using hexane-EtOAc-MeOH mixtures of increasing polarity, to afford 2.4 mg of the title compound (yield: 4%)

1. temperaturethe mixture was heated
2. temperatureto reflux overnight
3. temperatureto cool
4. concentrationconcentrated
5. additionThe residue was treated with saturated NaHCO3 and it
6. extractionwas extracted with CHCl3
7. dry with materialThe organic phase was dried over Na2SO4
8. concentrationconcentrated to dryness
9. customThe crude product obtained
10. customwas purified by chromatography on silica gel
11. temperatureof increasing polarity