反应详情

温度

65 °C

A mixture of 7-acetyl-5-fluoroquinolin-8-yl trifluoromethanesulfonate (3.4 g, 10. mmol, from Example 53, Step 2) in tetrahydrofuran (10 mL) was degassed for 10 minutes, to which was added tetrakis(triphenylphosphine)palladium(0) (1.2 g, 1.0 mmol) and 0.5 M (3-fluorophenyl)(iodo)zinc in tetrahydrofuran (50 mL). The reaction mixture was heated at 65° C. overnight, and then cooled to room temperature. The reaction was quenched with sat. NaHCO3 solution. The mixture was filtered through a Celite pad. The filtrate was extracted with dichloromethane. The combined organic layers were wash with brine, dried over MgSO4, concentrated and purified on silica gel (eluting with 0 to 30% ethyl acetate in hexane) to give the desired product (0.32 g, 11%). LCMS calculated for C17H12F2NO (M+H)+: m/z=284.1; Found: 284.1.

1. customwas degassed for 10 minutes, to which
2. temperaturecooled to room temperature
3. customThe reaction was quenched with sat. NaHCO3 solution
4. filtrationThe mixture was filtered through a Celite pad
5. extractionThe filtrate was extracted with dichloromethane
6. washThe combined organic layers were wash with brine
7. dry with materialdried over MgSO4
8. concentrationconcentrated
9. custompurified on silica gel (eluting with 0 to 30% ethyl acetate in hexane)