HRID649101

反应详情

EQUATION

反应方程式

HRID 649101 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

2,4,5-Trichlorophenol (20 g) in dry dimethylacetamide (40 ml) was treated with sodium hydride (5.28 g of 50% dispersion in oil) in portions and the resulting mixture heated to 120° C. Ethyl-5-chloro-2-nitrobenzoate (16.5 g) was added in solution in dry dimethylacetamide (60 ml) and the mixture heated at 160° C. for ten hours. The solvent was removed and the residue washed with water and extracted with ether. The ether solution was extracted with ether. The ether solution was evaporated. The remaining oil solidified and was recrystallised from ethanol to give ethyl 5(2,4,5-trichlorophenoxy)-2-nitrobenzoate (10.9 g) with a melting point of 99°-102° C.

WORKUP

后处理

  1. temperaturethe mixture heated at 160° C. for ten hours
  2. customThe solvent was removed
  3. washthe residue washed with water
  4. extractionextracted with ether
  5. extractionThe ether solution was extracted with ether
  6. customThe ether solution was evaporated
  7. customThe remaining oil solidified and was recrystallised from ethanol