反应详情

A mixture of 4-fluoro-3-nitrobenzoic acid (10.0 g; 54.0 mmol), SOCl2 (20.0 mL; 270 mmol) and DMF (2-3 drops) was refluxed for 4 h, concentrated and the residue was dissolved in DCM (25 mL) and slowly added to a mixture of 4-bromoaniline (9.3 g; 54.1 mmol) and TEA (11.4 mL; 81.0 mmol) in DCM (50 mL) at 0° C. The mixture was stirred for 1 h at rt, concentrated, EtOAc was added and the organic phase was washed with aqueous NaHCO3, aqueous HCl (1 M), dried over Na2SO4, filtered and concentrated to give the sub-title compound. Yield: 18.0 g (98%).

1. temperaturewas refluxed for 4 h
2. concentrationconcentrated
3. dissolutionthe residue was dissolved in DCM (25 mL)
4. concentrationconcentrated
5. additionEtOAc was added
6. washthe organic phase was washed with aqueous NaHCO3, aqueous HCl (1 M)
7. dry with materialdried over Na2SO4
8. filtrationfiltered
9. concentrationconcentrated