HRID2231213

反应详情

EQUATION

反应方程式

HRID 2231213 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a mixture of 9-chloro-2-(4-nitrophenyl)-4,4a,5,6-tetrahydrobenzo[h]cinnolin-3(2H)-one in ethanol and water is added iron powder with stirring at room temperature. To the mixture is added dropwise concentrated hydrochloric acid with stirring and heating up to 60° C. on a water bath. The resulting mixture is further stirred under heating at the same temperature and filtered, then the filtrate is concentrated. After the residue is made alkaline by adding an aqueous solution of sodium hydroxide, the mixture is extracted with chloroform. The extract is washed with water and dried over magnesium sulfate anhydride. The chloroform is distilled off to give 2-(4-aminophenyl)-9-chloro-4,4a,5,6-tetrahydrobenzo[h]cinnolin-3(2H)-one.

WORKUP

后处理

  1. stirringwith stirring
  2. temperatureheating up to 60° C. on a water bath
  3. stirringThe resulting mixture is further stirred
  4. temperatureunder heating at the same temperature
  5. filtrationfiltered
  6. concentrationthe filtrate is concentrated
  7. additionby adding an aqueous solution of sodium hydroxide
  8. extractionthe mixture is extracted with chloroform
  9. washThe extract is washed with water
  10. dry with materialdried over magnesium sulfate anhydride
  11. distillationThe chloroform is distilled off