反应详情

温度

-20 °C

0.5 g (1.4 mmol) of 3-(4-chloro-2-methylbenzofuran-7-yl)-1-methyl-6-trifluoromethyluracil was dissolved in 10 ml of concentrated sulfuric acid, and 0.1 g (1.1 mmol) of 60% nitric acid was dropwise added thereto at -20° C. After stirring at -20° C. for 10 minutes, the reaction solution was poured into ice water and extracted with 50 ml of chloroform. The organic layer was washed sequentially with water and a saturated sodium chloride aqueous solution and then dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure. Then, the obtained residue was purified by silica gel column chromatography to obtain 0.3 g (yield: 53.3%) of the desired product as a pale yellow crystals. Melting point: 174-175° C.

1. customat -20° C
2. extractionextracted with 50 ml of chloroform
3. washThe organic layer was washed sequentially with water
4. dry with materiala saturated sodium chloride aqueous solution and then dried over anhydrous magnesium sulfate
5. distillationThe solvent was distilled off under reduced pressure
6. customThen, the obtained residue was purified by silica gel column chromatography