反应详情

To a stirred suspension of 5.0 g (26 mmol) 2-Chloro-4,5-difluoro-benzoic acid (Apollo) and 50 ml methanol were added 7.41 ml (104 mmol) acetyl chloride drop wisely at 0° C. The reaction mixture was stirred over night, filtered and concentrated. The residue was diluted with dichloromethane, washed with diluted sodium hydrogen carbonate solution, dried with sodium sulphate and concentrated. The residue was purified by column chromatography (hexane:ethylacetate). The desired product 22a was obtained in 84% yield (4.51 g, 21.8 mmol).

1. customdrop wisely at 0° C
2. filtrationfiltered
3. concentrationconcentrated
4. additionThe residue was diluted with dichloromethane
5. washwashed with diluted sodium hydrogen carbonate solution
6. dry with materialdried with sodium sulphate
7. concentrationconcentrated
8. customThe residue was purified by column chromatography (hexane:ethylacetate)