HRID1156900

反应详情

EQUATION

反应方程式

HRID 1156900 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 22 g of 1-(4-methylphenyl)-5-chloroisoquinoline, 74.4 g of copper cyanide and 420 ml of hexamethylphosphotriamide was heated overnight under reflux. After the reaction, the reaction mixture was poured into a mixture of ethylenediamine, water and benzene, and stirred for 30 minutes. The mixture was then filtered through Celite. The benzene layer as filtrate was washed in water, and dried, followed by distilling off the solvent. The residue was recrystallized from ether to afford 16.4 g of 1-(4-methylphenyl)-5-cyanoisoquinoline as colorless needles having a melting point of 131.8° to 132.4° C.

WORKUP

后处理

  1. temperaturewas heated overnight
  2. temperatureunder reflux
  3. customAfter the reaction
  4. filtrationThe mixture was then filtered through Celite
  5. washThe benzene layer as filtrate was washed in water
  6. customdried
  7. distillationby distilling off the solvent
  8. customThe residue was recrystallized from ether