HRID2163685

反应详情

EQUATION

反应方程式

HRID 2163685 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

To a solution of 5.7 g. 2,2-dichloropropionic acid and 2.8 g. potassium carbonate in 40 ml water is added a solution of 6.9 g. phenethylhydrazine hydrochloride and 5.6 g. potassium carbonate in 20 ml water. The mixture is heated with stirring to 90° C., a further solution of 5.6 g. potassium carbonate in 20 ml water is dropped in over 30 minutes and further stirred for 60 minutes at 90° C. Afterwards the still alkaline solution is cooled to ambient temperature, shaken out with ether and acidified with concentrated hydrochloric acid. 2-(phenethylhydrazono)-propionic acid crystallizes out and is recrystallized from toluene. The yield is 3.3 g. (40% of theory); m.p. 74°-76° C.

WORKUP

后处理

  1. temperatureThe mixture is heated
  2. stirringfurther stirred for 60 minutes at 90° C
  3. temperatureAfterwards the still alkaline solution is cooled to ambient temperature
  4. custom2-(phenethylhydrazono)-propionic acid crystallizes out
  5. customis recrystallized from toluene