反应详情

温度

45 °C

To a mixture of sulfuric acid (0.27 ml) and nitric acid (0.34 ml), a solution of the compound (1.0 g) obtained in Example 561 in acetic acid (30 ml) was added dropwise at 5° C. The reaction mixture was stirred at 45° C. for 4 h, poured into ice cold water and ethyl acetate was added to the mixture. The organic layer was washed with a saturated aqueous sodium bicarbonate solution and a saturated aqueous sodium chloride solution, dried with anhydrous sodium sulfate and the solvent was distilled off under reduced pressure. The resulting residue was purified by silica gel column chromatography (eluent, n-hexane:ethyl acetate=9:1) to give 530 mg of the titled compound (yield, 46%).

1. additionwas added to the mixture
2. washThe organic layer was washed with a saturated aqueous sodium bicarbonate solution
3. dry with materiala saturated aqueous sodium chloride solution, dried with anhydrous sodium sulfate
4. distillationthe solvent was distilled off under reduced pressure
5. customThe resulting residue was purified by silica gel column chromatography (eluent, n-hexane:ethyl acetate=9:1)