反应详情

温度

40 °C

Concentrated hydrochloric acid (0.202 mL, 2.39 mmol) was added to a solution of 4-(1-ethoxy-vinyl)-N-(3-methoxy-4-(4-methyl-1H-imidazol-1-yl)phenyl)-6-(1-(2,2,2-trifluoroethoxy)ethyl)-pyrimidin-2-amine (0.38 g, 0.80 mmol) in dioxane (30 mL) and water (3 mL). The solution was heated at 40° C. for 0.5 h, cooled and neutralised with sodium bicarbonate (1 g). Brine was added (5 mL) and the water phase was extracted with ethyl acetate (2×10 mL). The organic phase was dried over sodium sulfate and concentrated. The residue was purified on silica gel column using a gradient 0-4% methanol in dichloromethane as eluent to give the title compound, 330 mg (92%).

1. extractionthe water phase was extracted with ethyl acetate (2×10 mL)
2. dry with materialThe organic phase was dried over sodium sulfate
3. concentrationconcentrated
4. customThe residue was purified on silica gel column