HRID2231215

反应详情

EQUATION

反应方程式

HRID 2231215 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-(4-Aminophenyl)-9-chloro-4,4a,5,6-tetrahydrobenzo[h]cinnolin-3(2H)-one is added to the mixture of water and concentrated hydrochloric acid which is cooled on an ice bath and then an aqueous solution of sodium nitrite is added dropwise. The mixture is stirred under ice-cooling for 30 minutes and then neutralized with sodium carbonate. The solution is added dropwise with stirring to a solution of cuprous cyanide and potassium cyanide which is previously prepared. The mixture is stirred under ice-cooling for 30 minutes and allowed to stand overnight at room temperature. The precipitated crystals are collected by filtration to give 9-chloro-2-(4-cyanophenyl)-4,4a,5,6-tetrahydrobenzo[h]cinnolin-3(2H)-one.

WORKUP

后处理

  1. temperatureis cooled on an ice bath
  2. temperaturecooling for 30 minutes
  3. additionThe solution is added dropwise
  4. customis previously prepared
  5. stirringThe mixture is stirred under ice-
  6. temperaturecooling for 30 minutes
  7. filtrationThe precipitated crystals are collected by filtration