反应详情

温度

85 °C

To a mixture of 2-chloroethyl (1R)-1-phenyl-1,2-dihydro[1,4]oxazino[2,3,4-jk]carbazol-7-yl ether in DMF (20 mL) is added sodium iodide (1.0 g, 6.7 mmol), potassium carbonate (2.0 g, 14.5 mmol), and ethanolamine (0.42 mL, 7.0 mmol). The mixture is heated to 85° C. for 18 h. The mixture then is partitioned between water and CH2Cl2. The layers are separated and the organic layer washed twice with water (200 mL). The organic layer is dried over anhydrous sodium sulfate, filtered and concentrated. Column chromatography with silica gel (60 mL) using CH3OH/CH2Cl2 (2/98) and then rechromatographed with CH3OH/CH2Cl2/NH4OH (4/96/0.1) gave 0.62 g (24%) of the title compound.

1. customThe mixture then is partitioned between water and CH2Cl2
2. customThe layers are separated
3. washthe organic layer washed twice with water (200 mL)
4. dry with materialThe organic layer is dried over anhydrous sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated
7. customrechromatographed with CH3OH/CH2Cl2/NH4OH (4/96/0.1)