HRID371471

反应详情

EQUATION

反应方程式

HRID 371471 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
140 °C

PROCEDURE

实验过程

A mixture of 20.5 g (0.10 mole) of 5-bromo-6-methyl-2,4(1H,3H)-pyrimidinedione, 18.1 g (0.10 mole) of 4-(4-cyanophenyl)piperazine, 6.4 g (0.11 mole) of anhydrous potassium fluoride, 15.2 g (0.1 mole) of powdered potassium carbonate in 100 ml of hexamethyl phosphoramide was heated at 140° C. for 24 hours. The mixture was cooled and poured into 500 ml of ice water. The solid was collected and washed with 100 ml of water. Recrystallization from N,N-dimethylformamide and drying in vacuo at 78° C. for 16 hours gave 9.3 g of the product as a dull solid.

WORKUP

后处理

  1. temperatureThe mixture was cooled
  2. customThe solid was collected
  3. washwashed with 100 ml of water
  4. customRecrystallization from N,N-dimethylformamide
  5. customdrying in vacuo at 78° C. for 16 hours