反应详情

To a mixture of 2-chloro-3,4-difluorobenzoic acid (2.50 g), 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (2.99 g), 1-hydroxybenztriazole (2.39 g) and N,N-dimethylformamide (72 mL) was added 28% aqueous ammonia (1.6 mL) at room temperature, and the mixture was stirred for 40 hr. 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). The obtained solid was washed with dichloromethane to give the title compound as a solid (yield: 1.30 g).

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)
6. washThe obtained solid was washed with dichloromethane