反应详情

温度

120 °C

A vial containing 2-chloro-4-(1-ethoxyvinyl)-6-((2,2,2-trifluoroethoxy)methyl)pyrimidine (0.29 g, 0.98 mmol), 3-methoxy-4-(4-methyl-1H-imidazol-1-yl)aniline (0.397 g, 1.96 mmol), cesium carbonate (0.637 g, 1.96 mmol), palladium(II) acetate (0.033 g, 0.15 mmol), 2-(dicyclohexylphosphino)biphenyl (0.051 g, 0.15 mmol) and dioxane (14 mL) was capped, evacuated and flushed with nitrogen. The mixture was heated by microwave irradiation at 120° C. for 1.5 h. The volatiles were removed in vacuum and the residue was extracted with ethyl acetate (20 mL). The solution was filtered through a short pad of silica gel, the pad was washed with ethyl acetate and 10% solution of methanol in ethyl acetate. The solvents were removed in vacuum and the residue was purified by column chromatography using a 0-5% gradient of methanol in dichloromethane to yield the title compound, 418 mg (92%).

1. customwas capped
2. customevacuated
3. customflushed with nitrogen
4. customThe volatiles were removed in vacuum
5. extractionthe residue was extracted with ethyl acetate (20 mL)
6. filtrationThe solution was filtered through a short pad of silica gel
7. washthe pad was washed with ethyl acetate and 10% solution of methanol in ethyl acetate
8. customThe solvents were removed in vacuum
9. customthe residue was purified by column chromatography