反应详情

To a mixture of AcOH (10 ml), conc. sulfuric acid (10 ml) and nitric acid (0.55 ml) was added by portions 1-acetyl-5-bromo-3-(2-ethoxy-carbonylethyl)-4,6-dimethylindoline (3.0 g) at 0° C., and the mixture was stirred at the same temperature for 5 hr. The reaction mixture was poured into ice water and extracted with CHCl3 (100 ml). After washing with water, the mixture was dried over anhydrous sodium sulfate. CHCl3 was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: CHCl3/MeOH=50/1−10/1) to give 2.7 g of 1-acetyl-5-bromo-3-(2-ethoxycarbonylethyl)-4,6-dimethyl-7-nitroindoline.

1. extractionextracted with CHCl3 (100 ml)
2. washAfter washing with water
3. dry with materialthe mixture was dried over anhydrous sodium sulfate
4. customCHCl3 was evaporated under reduced pressure
5. customThe residue was purified by silica gel column chromatography (eluent: CHCl3/MeOH=50/1−10/1)