HRID573630
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 80 °C
PROCEDURE
实验过程
A mixture of N-{2-bromo-6-methyl-3-[3-(methyloxy)phenyl]thieno[2,3-b]pyridin-4-yl}-3-chlorobenzenesulfonamide (70 mg, 0.134 mmol) (Example 33), 3-furanylboronic acid (22.43 mg, 0.20 mmol), sodium carbonate (28.3 mg, 0.267 mmol) and tetrakis(triphenylphosphine)palladium(0) (15.44 mg, 0.013 mmol) in acetonitrile (1 mL) and water (250 μl) was heated at 80° C. under nitrogen for 1.5 h. The reaction mixture was cooled to RT and concentrated. Purification by chromatography on silica gel, eluting with a gradient of 0-50% ethyl acetate in isohexane, afforded the title compound (55 mg). LCMS (A) m/z: 511 [M+1]+, Rt 1.51 min (acidic), Rt 0.98 min (basic).
WORKUP
后处理
- temperatureThe reaction mixture was cooled to RT
- concentrationconcentrated
- customPurification by chromatography on silica gel
- washeluting with a gradient of 0-50% ethyl acetate in isohexane