反应详情

8-Chloro-3,4-dihydro-1H-benzo[b]azepine-2,5-dione (iv-j) (0.2 g, 1 mmol) was dissolved in a mixture of THF (10 mL) and DMF (2 mL). Cesium carbonate (0.98 g, 3 mmol) and methyl iodide (0.069 mL, 1.1 mmol) were added and the reaction mixture was stirred at room temperature for 3 h. The mixture was concentrated under reduced pressure and dichloromethane (10 mL) was added. The inorganic precipitate was filtered and the filtrate was concentrated under reduced pressure to give a viscous residue. This residue was purified utilizing column chromatography, eluting with 50% ethyl acetate/hexane to afford the title compound as a white solid (0.1 g, 45%): MS m/z=224 (M+H).

1. concentrationThe mixture was concentrated under reduced pressure and dichloromethane (10 mL)
2. additionwas added
3. filtrationThe inorganic precipitate was filtered
4. concentrationthe filtrate was concentrated under reduced pressure
5. customto give a viscous residue
6. customThis residue was purified utilizing column chromatography
7. washeluting with 50% ethyl acetate/hexane