反应详情

3-(4Chloro-6-fluoro-3-methoxy-2-nitrophenyl)-6-trifluoromethyl-2,4(1H, 3H)-pyrimidinedione (9 g, 23.5 mmol) was dissolved in dimethylformamide (90 ml) and to this were added potassium carbonate (3.9 g, 28.2 mmol) and dimethylsulfate (10.2 g, 47 mmol) with stirring. The solution was stirred at ambient temperature for 12 hr and water was added. Product was extracted in ethyl acetate and the organic layer was washed with water and dried over anhydrous sodium sulfate. Removal of the solvent afforded a crude product which was purified by column chromatography on silica gel. Elution of the column with methylene chloride afforded the title compound (7.8 g).

1. stirringThe solution was stirred at ambient temperature for 12 hr
2. extractionProduct was extracted in ethyl acetate
3. washthe organic layer was washed with water
4. dry with materialdried over anhydrous sodium sulfate
5. customRemoval of the solvent
6. customafforded a crude product which
7. customwas purified by column chromatography on silica gel
8. washElution of the column with methylene chloride