反应详情

温度

80 °C

A mixture of methyl 4-bromo-2-fluorobenzoate (7.0 g, 0.030 mol), 1-(ethenyloxy)butane (13 mL, 0.099 mol), palladium acetate (200 mg, 0.0009 mol), 1,3-bis(diphenylphosphino)propane (700 mg, 0.002 mol), and potassium carbonate (4.29 g, 0.0310 mol) in DMF (50 mL) and water (3 mL) was heated at 80° C. with stirring for 24 h. After cooling to RT, to the solution was added 1N HCl solution (31 ml). The mixture was stirred at RT for 1 h, and then extracted with ethyl ether. The combined extracts were washed with brine; dried over Na2SO4, filtered concentrated. The residue was flash chromatographed on a silica gel column to give the desired product (1.64 g).

1. temperatureAfter cooling to RT, to the solution
2. stirringThe mixture was stirred at RT for 1 h
3. extractionextracted with ethyl ether
4. washThe combined extracts were washed with brine
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated
8. customchromatographed on a silica gel column