反应详情

To a solution of sodium metaperiodate (1.200 g, 5.61 mmol) and 4-(1-ethoxyvinyl)-N-(3-methoxy-4-(4-methyl-1H-imidazol-1-yl)phenyl)-6-((2,2,2-trifluoroethoxy)methyl)pyrimidin-2-amine (1.3 g, 2.81 mmol) in a mixture of water (30 mL) and 1,4-dioxane (60 mL) potassium permanganate (0.066 g, 0.42 mmol) was added in portions of 10-15 mg in intervals of 5-8 min at ambient temperature. The mixture was filtered, the precipitate was washed with dioxane and ethyl acetate. Sodium bicarbonate and sodium chloride were added to the filtrate, the organic phase was separated, and the water phase was additionally extracted with ethyl acetate. The combined organic phase was dried over sodium sulfate and concentrated in vacuum. The residue was separated on a silica gel column using a gradient of 0-5% methanol in dichloromethane as eluent to yield the title product, 0.96 g (74%).

1. additionwas added in portions of 10-15 mg in intervals of 5-8 min at ambient temperature
2. filtrationThe mixture was filtered
3. washthe precipitate was washed with dioxane and ethyl acetate
4. additionSodium bicarbonate and sodium chloride were added to the filtrate
5. customthe organic phase was separated
6. extractionthe water phase was additionally extracted with ethyl acetate
7. dry with materialThe combined organic phase was dried over sodium sulfate
8. concentrationconcentrated in vacuum
9. customThe residue was separated on a silica gel column