反应详情

To a solution of compound 3-bromo-4-fluoro-benzoic acid (430 g, 1.97 mol, 1 eq) in EtOH (2.3 L) was added dropwise thionyl chloride (287 mL, 3.94 mol, 2 eq) at 10° C. Then the mixture was heated to reflux overnight. The mixture was concentrated in vacuum to give a residue. The residue was dissolved in ethyl acetate (800 mL), washed with aqueous sodium hydrogen carbonate, brine (300 mL) and water (200 mL), then concentrated in vacuo to give title compound as a white solid (440 g, 1.78 mol, 90.3%).

1. temperatureThen the mixture was heated
2. temperatureto reflux overnight
3. concentrationThe mixture was concentrated in vacuum
4. customto give a residue
5. washwashed with aqueous sodium hydrogen carbonate, brine (300 mL) and water (200 mL)
6. concentrationconcentrated in vacuo