反应详情

温度

0 °C

2-(4-Methoxy-benzyl)-4,4-dimethyl-7-nitro-3,4-dihydro-2H-isoquinolin-1-one (2.0 g) was dissolved in CH3CN (100 ml) and H2O (50 ml) and cooled to 0° C. CAN (9.64 g) was added and the reaction was stirred at 0° C. for 30 min, then warmed to RT and stirred for 6 h. The mixture was extracted with CH2Cl2 (2×300 ml) washed with sat'd NH4Cl, dried over MgSO4, filtered and concentrated. The crude material was recrystallized in CH2Cl2/EtOAc (1:1) to give 4,4-dimethyl-7-nitro-3,4-dihydro-2H-isoquinolin-1-one as a white solid.

1. temperaturewarmed to RT
2. stirringstirred for 6 h
3. extractionThe mixture was extracted with CH2Cl2 (2×300 ml)
4. washwashed with sat'd NH4Cl
5. dry with materialdried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated
8. customThe crude material was recrystallized in CH2Cl2/EtOAc (1:1)