反应详情

Sodium metaperiodate (2.111 g, 9.87 mmol) was suspended in water (20 mL) and sonicated until a clear solution was obtained. 2,4-Dichloro-6-(1-ethoxyvinyl)-5-methylpyrimidine (1.15 g, 4.93 mmol) dissolved in 1,4-dioxane (40 mL) was added followed by potassium permanganate (0.117 g, 0.74 mmol). The mixture was stirred at rt for 2 h. The mixture was filtered. The filtrate was diluted with saturated solutions of sodium bicarbonate and sodium chloride and extracted twice with ethyl acetate. The organic phase was dried over sodium sulfate, filtered through a pad of silica gel and concentrated in vacuum. Column chromatography on silica gel using a 0-30% gradient of ethyl acetate in heptane yielded the title product, 0.67 g (58%).

1. customsonicated until a clear solution
2. customwas obtained
3. additionwas added
4. filtrationThe mixture was filtered
5. additionThe filtrate was diluted with saturated solutions of sodium bicarbonate and sodium chloride
6. extractionextracted twice with ethyl acetate
7. dry with materialThe organic phase was dried over sodium sulfate
8. filtrationfiltered through a pad of silica gel
9. concentrationconcentrated in vacuum