HRID261510

反应详情

EQUATION

反应方程式

HRID 261510 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customwas effected at 80° C. under a nitrogen
  2. customfor 1 hour
  3. distillationThe ethanol was distilled off under reduced pressure
  4. additionthe residual liquid was diluted with 100 ml of cold water
  5. extractionThe solid thus deposited was extracted with ether
  6. extractionthe ether extract
  7. washwas washed with water
  8. dry with materialdried over anhydrous sodium sulfate
  9. distillationthe ether was distilled off at room temperature under reduced pressure
  10. customThe residue was recrystallized from ether-petroleum ether