HRID637554

反应详情

EQUATION

反应方程式

HRID 637554 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

To an autoclave there are added 30.7 g (0.1 moles) of 4-chloro-3,4'-dinitro benzophenone, 10.6 g (0.1 moles) of sodium carbonate, 1 g of 5% palladium/alumina catalyst (available from Nihon-Engelhardt Co.) and 250 ml of 1,2-dichloro ethane. With the mixture being stirred at 30°-35° C., the reaction is carried out at a constant pressure for 10 hours by introducing hydrogen into the mixture. After completion of the reaction, the reaction mixture is heated up to 70° C. to be subjected to filtering for removing the catalyst. Then, on cooling, there is obtained 3,4'-diamino benzophenone in the form of yellow needle-like crystals. The crystals are filtered, washed with 20 ml of 1,2-dichloro ethane and dried. Yield 17.6 g (83%). M.P. 121°-122° C. Recrystallization from ethanol gives yellow needle-like pure crystals of said benzophenone. M.P. 122°-122.5° C.

WORKUP

后处理

  1. customAfter completion of the reaction
  2. filtrationto filtering
  3. customfor removing the catalyst
  4. temperatureThen, on cooling