HRID358048

反应详情

EQUATION

反应方程式

HRID 358048 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

100 g of 2-amino-2'-chloro-5-nitrobenzophenone are suspended in 865 ml of 25% hydrochloric acid and treated portionwise with a total of 269 g of tin (II) chloride. The mixture is stirred at room temperature for 36 hours, then diluted with 0.5 l of an ice/water mixture and adjusted to pH 10 with about 2.17 l of a 28% sodium hydroxide solution. The mixture is extracted with methylene chloride. After evaporation of the solvent, the residue is dissolved in 0.54 l of ether and crystallized at about -20°. There is obtained 2,5-diamino-2'-chlorobenzophenone of melting point 30°-40°.

WORKUP

后处理

  1. extractionThe mixture is extracted with methylene chloride
  2. customAfter evaporation of the solvent
  3. dissolutionthe residue is dissolved in 0.54 l of ether
  4. customcrystallized at about -20°