反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customThe vial was capped
- customevacuated
- customflushed with nitrogen
- temperaturecooled
- filtrationfiltered through a pad of silica gel
- washThe pad was eluted with 10% methanol in ethyl acetate
- customThe solvents were evaporated
- customthe residue was purified by column chromatography on silica gel using a gradient of 0-10% methanol in dichloromethane as eluent