反应详情

温度

60 °C

To a solution of 5-[2-(methylsulfonyl)pyrimidin-4-yl]-6-[3-(trifluoromethyl)phenyl]-1H-pyrazolo[3,4-b]pyridine (90 mg, 0.2 mmol, obtained in example 127) in MeOH (5 mL) in a closed vessel, sodium methoxide (11 mg, 0.2 mmol) was added and heated to 60° C. for 24 h. Then, sodium methoxide (11 mg, 0.2 mmol) was added and it was stirred at 60° C. for 2 h more. It was allowed to cool and was concentrated. EtOAc and buffer (pH=5.3) were added. The phases were separated and the organic phase was washed with water, dried over Na2SO4 and concentrated to dryness. The crude product obtained was purified by chromatography on silica gel using hexane-EtOAc mixtures at 50%, to afford 38 mg of the title compound (yield: 47%)

1. temperatureto cool
2. concentrationwas concentrated
3. additionEtOAc and buffer (pH=5.3) were added
4. customThe phases were separated
5. washthe organic phase was washed with water
6. dry with materialdried over Na2SO4
7. concentrationconcentrated to dryness
8. customThe crude product obtained
9. customwas purified by chromatography on silica gel