反应详情

温度

120 °C

To a suspension of Pd(PPh3)4 (1.27 g, 1.1 mmol) and sodium formate (13.8 g, 132 mmol, 6 e.q.) in acetonitrile (30 mL) was added a solution of 6-bromo-7-fluoro quinoline (5 g, 22 mmol) in DMSO (30 mL). The reaction mixture was heated at 120° C. under a CO atmosphere (1 MPa) for 4 h, cooled to rt and concentrated under reduced pressure. The residue was partitioned between water (100 mL) and ethyl acetate (150 mL). The organic layer was separated, washed with brine (100 mL), dried over Na2SO4 and concentrated under reduced pressure. The reside was purified by column choromatography, eluting with petroleum:ethyl acetate=10:1˜3:1 to give the title compound as a white solid (400 mg, 10.4%). 1H-NMR (400 MHz, DMSO-d6) δ ppm 8.95 (s, 1H), 8.46 (m, 1H), 8.20 (m, 1H), 7.75 (d, 1H), 7.53 (m, 1H).

1. temperaturecooled to rt
2. concentrationconcentrated under reduced pressure
3. customThe residue was partitioned between water (100 mL) and ethyl acetate (150 mL)
4. customThe organic layer was separated
5. washwashed with brine (100 mL)
6. dry with materialdried over Na2SO4
7. concentrationconcentrated under reduced pressure
8. customThe reside was purified by column choromatography
9. washeluting with petroleum