反应详情

温度

60 °C

To a solution of 4-methoxyisoquinoline (130 mg, 0.82 mmol) in 98% sulfuric acid (0.61 mL) was added potassium nitrate (91 mg, 0.90 mmol), and the mixture was heated to 60° C. and stirred for 2 hours. The reaction solution was cooled, and then thereto was added ice. The powders were filtered to dissolve in ethyl acetate. The solution was washed with aqueous sodium hydrogen carbonate solution and saturated brine, and then dried over anhydrous sodium sulfate, followed by concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=9:1→2:8) to give 4-methoxy-3-nitroisoquinoline (58.3 mg, 35%) as a pale yellow powder.

1. temperatureThe reaction solution was cooled
2. additionwas added ice
3. filtrationThe powders were filtered
4. dissolutionto dissolve in ethyl acetate
5. washThe solution was washed with aqueous sodium hydrogen carbonate solution and saturated brine
6. dry with materialdried over anhydrous sodium sulfate
7. concentrationby concentrated under reduced pressure
8. customThe resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=9:1→2:8)