反应详情

温度

95 °C

A mixture of 1-[1-(3-bromo-5-chloro-2-methoxy-4-methylphenyl)ethyl]-3-methyl-1H-pyrazolo[3,4-d]pyrimidin-4-amine (peak 1 from Example 167, step 4, 322 mg, 0.76 mmol), 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridine-2-carbonitrile (210 mg, 0.91 mmol, from Combi-Blocks Catalog, item # PN-0143), sodium carbonate (130 mg, 1.2 mmol) and [1,1′-bis(diphenylphosphino)ferrocene]-dichloropalladium(II), complex with dichloromethane (1:1) (99 mg, 0.12 mmol) in acetonitrile (5 mL)/water (2 mL) was degassed with N2 and the reaction was stirred at 95° C. for 2 h. The mixture was diluted with methylene chloride, washed with sat. NaHCO3, water, brine, dried over Na2SO4, filtered and concentrated. The product (0.28 g, 85%) was purified by chromatography eluting with CH2Cl2/MeOH (max. MeOH 6%). LCMS calculated for C22H21ClN7O (M+H)+: m/z=434.1; Found: 434.1

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 (0.28 g, 85%) was purified by chromatography
8. washeluting with CH2Cl2/MeOH (max. MeOH 6%)