HRID573623

反应详情

EQUATION

反应方程式

HRID 573623 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

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 (50 mg, 0.095 mmol) (Example 33), tetrakis(triphenylphosphine)palladium(0) (5.51 mg, 4.77 μmol), sodium carbonate (20.23 mg, 0.191 mmol) and 3-pyridineboronic acid (14.08 mg, 0.115 mmol) in acetonitrile (1 mL) and water (250 μl) was heated at 80° C. under nitrogen for 17 h. The reaction mixture was then cooled to RT and concentrated. Purification by chromatography on silica gel, eluting with a gradient of 0-50% ethyl acetate in DCM, afforded the title compound (20.5 mg). LCMS (A) m/z: 522 [M+1]+, Rt 1.33 min (acidic), Rt 0.89 min (basic).

WORKUP

后处理

  1. temperatureThe reaction mixture was then cooled to RT
  2. concentrationconcentrated
  3. customPurification by chromatography on silica gel
  4. washeluting with a gradient of 0-50% ethyl acetate in DCM