反应详情

温度

50 °C

To a stirred solution of (3R)-3-ethyl-6-fluoro-4-(4-methoxybenzoyl)-3,4-dihydroquinoxalin-2(1H)-one (0.20 g, 0.61 mmol) in acetonitrile (5 mL) under nitrogen was added potassium carbonate (0.050 g, 0.36 mmol), cesium carbonate (0.11 g, 0.33 mmol) and iodoethane (0.15 mL, 0.29 g, 1.9 mmol). The reaction was stirred for 10 h at 50° C. and then 5 h at 63° C. The solvent was evaporated, and the residue was partitioned between ethyl acetate and water. The layers were separated and the organic layer was washed with water. The organic layer was concentrated in vacuo and purified via Biotage Horizon® (SiO2, gradient from 5% EtOAc/hexane to 33% EtOAc/hexane) to yield 0.21 g (96%) of (3R)-1,3-diethyl-6-fluoro-4-(4-methoxybenzoyl)-3,4-dihydroquinoxalin-2(1H)-one. MS (ESI) m/z 357 ([M+H]+); HRMS: calcd for C20H21FN2O3, 356.16090; found (ESI+), 357.16057.

1. custom5 h
2. customat 63° C
3. customThe solvent was evaporated
4. customthe residue was partitioned between ethyl acetate and water
5. customThe layers were separated
6. washthe organic layer was washed with water
7. concentrationThe organic layer was concentrated in vacuo
8. custompurified via Biotage Horizon® (SiO2, gradient from 5% EtOAc/hexane to 33% EtOAc/hexane)