反应详情

To a mixture of 2-chloro-3,4-difluorobenzamide (1.20 g), pyridine (1.01 mL) and N,N-dimethylformamide (18 mL) was added oxalyl chloride (0.82 mL) at 0° C. over 10 min. The mixture was stirred for 1 hr while raising the temperature to room temperature. The reaction mixture was poured into water and extracted with ethyl acetate. The organic layer was washed with water, dried over anhydrous sodium sulfate and concentrated. The obtained residue was purified by silica gel column chromatography (developing solvent: ethyl acetate-hexane) to give the title compound as a solid (yield: 983 mg).

1. extractionextracted with ethyl acetate
2. washThe organic layer was washed with water
3. dry with materialdried over anhydrous sodium sulfate
4. concentrationconcentrated
5. customThe obtained residue was purified by silica gel column chromatography (developing solvent: ethyl acetate-hexane)