反应详情

温度

95 °C

A mixture of 4-amino-1-[1-(3-bromo-5-chloro-2-methoxy-4-methylphenyl)ethyl]-1H-pyrazolo[3,4-d]pyrimidine-3-carbaldehyde (20 mg, 0.047 mmol), {6-[(dimethylamino)carbonyl]pyridin-3-yl}boronic acid (23 mg, 0.12 mmol), sodium carbonate (10 mg, 0.094 mmol) and [1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium(II), complex with dichloromethane (1:1) (7.7 mg, 0.0094 mmol) in acetonitrile (0.3 mL)/ethanol (0.1 mL)/water (0.1 mL) was degassed with N2 and then stirred at 95° C. for 3 h. The mixture was diluted with methylene chloride, washed with sat. NaHCO3, water, brine, dried over Na2SO4, filtered and concentrated. The product was purified by chromatography eluting with CH2Cl2/MeOH (max. MeOH 6%). LCMS calculated for C24H25ClN7O3 (M+H)+: m/z=494.2; Found: 494.1

1. customwas degassed with N2
2. additionThe mixture was diluted with methylene chloride
3. washwashed with sat. NaHCO3, water, brine
4. dry with materialdried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated
7. customThe product was purified by chromatography
8. washeluting with CH2Cl2/MeOH (max. MeOH 6%)