HRID1656929

反应详情

EQUATION

反应方程式

HRID 1656929 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
190 °C

PROCEDURE

实验过程

30 g of 1-chloro-2-methyl-3-prop-2-enylbenzene are dissolved in 150 ml of N-methylpyrrolidone, and 25 g of copper(I) cyanide are added. The reaction mixture is heated at 190° C. for 30 hours while stirring. After the mixture has been cooled to 20° C., 125 ml of ethylenediamine and 300 ml of water are added. Stirring is then carried out for 1 hour at 50° C. and for 14 hours at 20° C. Working up is effected by extracting with diethyl ether, washing the organic phase and drying over sodium sulfate, removing the drying agent and distilling off the organic solvent. 24.5 g of crude product are obtained. After chromatography (silica gel/toluene), 14.4 g of pure 1-cyano-2-mehtyl-3-prop-2-enylbenzene are isolated.

WORKUP

后处理

  1. temperatureAfter the mixture has been cooled to 20° C.
  2. stirringStirring
  3. extractionby extracting with diethyl ether
  4. washwashing the organic phase
  5. dry with materialdrying over sodium sulfate
  6. customremoving the drying agent
  7. distillationdistilling off the organic solvent
  8. custom24.5 g of crude product are obtained