HRID2413957

反应详情

EQUATION

反应方程式

HRID 2413957 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

86 g (1.00 mole) of β-butyrolactone was added to 162 g (1.00 mole) of 3,4-dichloroaniline, and this mixture was stirred at 110°-120° C. for 1 hour and then allowed to cool to room temperature. To the resulting reaction solution was added 1000 ml of ether. This mixture was filtered to remove any insoluble matter, and the filtrate thus obtained was extracted with 750 ml of a 2N aqueous solution of sodium hydroxide. This extract was acidified with 130 ml of concentrated hydrochloric acid and then extracted with 1000 ml of ether. The ether layer was separated, dried over anhydrous sodium sulfate and then evaporated to dryness. Thus, there was obtained 128 g (51.6% yield) of 3-(3,4-dichloroanilino) butyric acid in the form of pale-yellow crystals.

WORKUP

后处理

  1. customTo the resulting reaction solution
  2. filtrationThis mixture was filtered
  3. customto remove any insoluble matter
  4. customthe filtrate thus obtained
  5. extractionwas extracted with 750 ml of a 2N aqueous solution of sodium hydroxide
  6. extractionextracted with 1000 ml of ether
  7. customThe ether layer was separated
  8. dry with materialdried over anhydrous sodium sulfate
  9. customevaporated to dryness