HRID231559

反应详情

EQUATION

反应方程式

HRID 231559 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

In a variant of (b), into a toluene solution of 33.3 g (0.3 moles) 4-fluoroaniline, a toluene solution of 44.6 g (0.3 moles) 2-chloromethylsuccinic acid anhydride were added dropwise at room temperature while stirring. The temperature of the mixture rose to 40° C. during the operation. To the suspension of the semi-anilide obtained, 0.35 moles of acetylchloride was added dropwise at 60° C. while stirring, the addition being carried out so slowly that the ensuing gas development could be easily controlled. After 3 hours the reaction mixture was heated to 100° C. and held at that temperature until the gas development was terminated. The semi-anilide thereby dissolved. When the reaction mixture was cooled down, the desired product crystallized. The actual yield was 93% of the theoretical yield.

WORKUP

后处理

  1. customrose to 40° C. during the operation
  2. customobtained
  3. stirringwhile stirring
  4. additionthe addition
  5. customwas terminated
  6. dissolutionThe semi-anilide thereby dissolved
  7. temperatureWhen the reaction mixture was cooled down
  8. customthe desired product crystallized