反应详情

To an ice-cooled mixture consisting of 0.8 g of 2-amino-5-ethoxycarbonyl-4,6-dimethylbenzoic acid, 20 ml of dry benzene, and 0.5 ml of pyridine was added dropwise with stirring a solution of 0.4 ml of chloroacetyl chloride in 5 ml of benzene. The mixture was stirred overnight and then, shaken with dilute hydrochloric acid. The layers were separated. The aqueous layer was extracted with ethyl acetate, and the combined organic extracts were washed with water, dried over sodium sulfate, and evaporated. The residue was recrystallized from ethyl ether/n-hexane to give 0.65 g of 2-chloroacetylamino-5-ethoxycarbonyl-4,6-dimethylbenzoic acid (m.p. 124°-125° C.).

1. additionwas added dropwise
2. customThe layers were separated
3. extractionThe aqueous layer was extracted with ethyl acetate
4. washthe combined organic extracts were washed with water
5. dry with materialdried over sodium sulfate
6. customevaporated
7. customThe residue was recrystallized from ethyl ether/n-hexane