HRID59067

反应详情

EQUATION

反应方程式

HRID 59067 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

2-Chloro-4-(1-ethoxyvinyl)-6-(1-(2,2,2-trifluoroethoxy)ethyl)pyrimidine (0.35 g, 1.13 mmol), 3-methoxy-4-(4-methyl-1H-imidazol-1-yl)aniline (0.275 g, 1.35 mmol), palladium(II) acetate (0.038 g, 0.17 mmol), 2-(dicyclohexylphosphino)biphenyl (0.059 g, 0.17 mmol), cesium carbonate (0.734 g, 2.25 mmol) and dioxane (4 mL) were mixed in a vial. The vial was capped, evacuated and flushed with nitrogen. The reaction mixture was heated by microwave irradiation at 120° C. for 2.5 h, cooled and filtered through a pad of silica gel. The pad was eluted with 10% methanol in ethyl acetate. The solvents were evaporated and the residue was purified by column chromatography on silica gel using a gradient of 0-10% methanol in dichloromethane as eluent to yield the title product, 0.38 mg (70%).

WORKUP

后处理

  1. customThe vial was capped
  2. customevacuated
  3. customflushed with nitrogen
  4. temperaturecooled
  5. filtrationfiltered through a pad of silica gel
  6. washThe pad was eluted with 10% methanol in ethyl acetate
  7. customThe solvents were evaporated
  8. customthe residue was purified by column chromatography on silica gel using a gradient of 0-10% methanol in dichloromethane as eluent