HRID65731

反应详情

EQUATION

反应方程式

HRID 65731 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

8.1 g of 2,3-Dichloroaniline (0.05 mole) in acetone (100 ml.) and concentrated hydrobromic acid (16 ml.) was stirred at -5° C. and treated with a solution of 4.2 g. of sodium nitrite (0.06 mole) in water (10 ml.). Methyl acrylate (0.5 mole) (43 g.) and cuprous bromide (100 mg.) were then added at 0° C. The reaction temperature was kept below 15° C. until nitrogen evolution ceased and then stirred at 25° C. for thirty minutes. The reaction mixture was poured into water and extracted with benzene which was dried over sodium sulfate and evaporated to give methyl 2-bromo-3-(2,3-dichlorophenyl)propionate. The propionate, 156 g. (0.5 mole) was dissolved in glacial acetic acid (1 l.) and stirred. Zinc dust 65 g. (1 mole) was added in portions and the mixture was stirred for one hour, filtered and evaporated to give methyl 3-(2,3-dichlorophenyl)propionate.

WORKUP

后处理

  1. additiontreated with a solution of 4.2 g
  2. customwas kept below 15° C. until nitrogen evolution
  3. extractionextracted with benzene which
  4. dry with materialwas dried over sodium sulfate
  5. customevaporated