HRID1905962

反应详情

EQUATION

反应方程式

HRID 1905962 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

6.1 g of phenethyl alcohol in 100 ml of dimethylformamide were treated with 4.8 g of a 50% sodium hydride dispersion in mineral oil and the mixture was stirred for 10 minutes at 60° C. 4.73 g of chloroacetic acid were added and the mixture was heated at 60° C. for 0.5 hour with stirring. The mixture was evaporated to dryness and the residue was partitioned between water and diethyl ether. The aqueous phase was acidified to pH 1 with concentrated hydrochloric acid and extracted with ethyl acetate. The organic phase was washed with water, dried over sodium sulfate, filtered and evaporated to dryness. The residue was recrystallized from ethyl acetate/hexane to give 7.65 g (85%) of 2-phenylethoxyacetic acid of melting point 46°-48° C.

WORKUP

后处理

  1. temperaturethe mixture was heated at 60° C. for 0.5 hour
  2. stirringwith stirring
  3. customThe mixture was evaporated to dryness
  4. customthe residue was partitioned between water and diethyl ether
  5. extractionextracted with ethyl acetate
  6. washThe organic phase was washed with water
  7. dry with materialdried over sodium sulfate
  8. filtrationfiltered
  9. customevaporated to dryness
  10. customThe residue was recrystallized from ethyl acetate/hexane