反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of 13.0 g of methyl 2-(2,6-dichloroanilino)-phenylglycolate in 150 ml of ethanol were added 10 ml of a 5 N aqueous sodium hydroxide solution and the reaction was effected at 80° C. under a nitrogen stream for 1 hour. The ethanol was distilled off under reduced pressure and the residual liquid was diluted with 100 ml of cold water and acidified with a 10% aqueous hydrochloric acid solution. The solid thus deposited was extracted with ether, and the ether extract was washed with water, dried over anhydrous sodium sulfate and then the ether was distilled off at room temperature under reduced pressure. The residue was recrystallized from ether-petroleum ether to give 10.1 g of 2-(2,6-dichloroanilino)phenylglycolic acid. m.p. 140°-142° C. Yield: 81% of theoretical amount.
WORKUP
后处理
- customwas effected at 80° C. under a nitrogen
- customfor 1 hour
- distillationThe ethanol was distilled off under reduced pressure
- additionthe residual liquid was diluted with 100 ml of cold water
- extractionThe solid thus deposited was extracted with ether
- extractionthe ether extract
- washwas washed with water
- dry with materialdried over anhydrous sodium sulfate
- distillationthe ether was distilled off at room temperature under reduced pressure
- customThe residue was recrystallized from ether-petroleum ether