HRID371458

反应详情

EQUATION

反应方程式

HRID 371458 反应方程式

CONDITIONS

反应条件

温度
130 °C

PROCEDURE

实验过程

A mixture of 5.0 g (0.016 mole) of 5-[4-(4-cyanophenyl)-1-piperazinyl]-6-methyl-2,4-pyrimidinediamine, 30 ml of 95% ethanol and 30 ml of sulfuric acid was heated under reflux at 130° C. for four hours and cooled. The solution was poured into 400 g of ice. The solid was collected, washed first with 5N aqueous sodium carbonate solution and then with 50 ml of water. Recrystallization from N,N-dimethylformamide gave 1.72 g of the product as an off-white solid, mp 281°-285° C.

WORKUP

后处理

  1. temperaturewas heated
  2. temperaturecooled
  3. customThe solid was collected
  4. washwashed first with 5N aqueous sodium carbonate solution
  5. customRecrystallization from N,N-dimethylformamide