反应详情

To a stirred solution of 4-amino-3-iodo-benzoic acid methyl ester (11.1 g, 40.0 mmol) in anhydrous pyridine (80 mL) was added acetyl chloride (3.30 g, 42.0 mmol) at 0° C. under nitrogen. Stirring was continued at 0° C. for 30 minutes. The ice-bath was removed, and stirring continued at room temperature for 16 hours. Pyridine was evaporated under reduced pressure. The residue was taken in ethyl acetate (300 mL). The organic phase washed with 2 N aqueous HCl (200 mL), water (200 mL), brine (200 mL), and was dried over anhydrous Na2SO4. Removal of solvent gave 4-acetylamino-3-iodo-benzoic acid methyl ester as a white solid. Yield: 12.7 g (99%).

1. customThe ice-bath was removed
2. stirringstirring
3. waitcontinued at room temperature for 16 hours
4. customPyridine was evaporated under reduced pressure
5. washThe organic phase washed with 2 N aqueous HCl (200 mL), water (200 mL), brine (200 mL)
6. dry with materialwas dried over anhydrous Na2SO4
7. customRemoval of solvent