反应详情

温度

80 °C

To a mixture of 1-phenyl-1,2-dihydro[1,4]oxazino[2,3,4-jk]carbazol-7-ol (0.82 g, 2.7 mmol) in dry DMF (12 mL) is added 1-bromo-3chloropropane (1.28 g, 8.1 mmol) and potassium carbonate (1.12 g, 8.1 mmol). The mixture is heated at 80° C. for 6 h. The mixture is then stirred at room temperature for 18 h followed by another 6 h at 80° C. The mixture is partitioned between water and CH2Cl2. The organic layer is washed 3 times with water (100 mL). The organic layer is then dried over anhydrous sodium sulfate and concentrated. Column chromatography (60 mL silica) using hexanes/CH2Cl2 (1:1) as eluent gave an oil which is rechromatographed (60 mL silica) using hexanes/CH2C]2 (60/40) as eluent gave 0.454 g (44%) of the title compound.

1. waitfollowed by another 6 h at 80° C
2. customThe mixture is partitioned between water and CH2Cl2
3. washThe organic layer is washed 3 times with water (100 mL)
4. dry with materialThe organic layer is then dried over anhydrous sodium sulfate
5. concentrationconcentrated
6. customgave an oil which
7. customis rechromatographed (60 mL silica)