反应详情

Sodium metaperiodate (701 mg, 3.28 mmol) was suspended in water (10 mL) and sonicated until a clear solution was obtained. 2-Chloro-4-(1-ethoxyvinyl)-6-((2,2,2-trifluoroethoxy)methyl)pyrimidine (486 mg, 1.64 mmol) in 1,4-dioxane (20 mL) and potassium permanganate (39 mg, 0.25 mmol) were added and the mixture was stirred at rt for 30 min. The mixture was filtered, precipitate was washed by dioxane and DCM. DCM an solid sodium bicarbonate (s) were added to the filtrate. The mixture was extracted with DCM (×2). The organic phase was dried over sodium sulfate and concentrated. The residue was purified by column chromatography on silica eluting with DC ti give the title compound as a solid, 385 mg (79%).

1. customsonicated until a clear solution
2. customwas obtained
3. filtrationThe mixture was filtered
4. washprecipitate was washed by dioxane and DCM
5. additionDCM an solid sodium bicarbonate (s) were added to the filtrate
6. extractionThe mixture was extracted with DCM (×2)
7. dry with materialThe organic phase was dried over sodium sulfate
8. concentrationconcentrated
9. customThe residue was purified by column chromatography on silica eluting with DC ti