HRID441847

反应详情

EQUATION

反应方程式

HRID 441847 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

A solution of 15.2 g. of sodium nitrite in 40 ml. of water is added dropwise to a solution at 0° C. of 21.4 g. of p-toluidine and 400 ml. of 7.5% hydrochloric acid. The suspension of p-toluene diazonium chloride obtained is added dropwise at 5° C. to a mixture consisting of 36.2 g. of 2-chloroacetic acid ethyl ester, 400 ml. of 50% ethanol and 164 g. of sodium acetate. The mixture then is stirred for three hours at 20° C. and extracted with ethyl acetate. The organic phase is concentrated and the residue is treated with petroleum ether. 41 g. of 2-chloro-2-(4-methyl-phenylhydrazono)-acetic acid ethyl ester with a melting point of 100°-101° C., is obtained.

WORKUP

后处理

  1. customobtained
  2. additionis added dropwise at 5° C. to a mixture
  3. extractionextracted with ethyl acetate
  4. concentrationThe organic phase is concentrated
  5. additionthe residue is treated with petroleum ether