HRID249976

反应详情

EQUATION

反应方程式

HRID 249976 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

6-Bromo-7-methoxy-3H-quinazolin-4-one (1.01 g, 3.96 mmol) and N,N-(diisopropyl-ethylamine (1.78 ml, 10.4 mmol) are introduced into 1,2-dichloroethane (19 ml), treated dropwise with POCl3 (0.46 ml, 4.95 mmol) and then stirred at 80° C. for 2 h. The reaction mixture is subsequently concentrated to dryness. The residue is taken up in isopropanol (10 ml), treated with isopropylamine (0.34 ml, 3.96 mmol) and stirred for 30 minutes at 80° C. After cooling to room temperature, the resulting precipitate is filtered off with suction and dried in vacuo. The desired product is obtained in 46% yield (530 mg).

WORKUP

后处理

  1. concentrationThe reaction mixture is subsequently concentrated to dryness
  2. stirringstirred for 30 minutes at 80° C
  3. temperatureAfter cooling to room temperature
  4. filtrationthe resulting precipitate is filtered off with suction
  5. customdried in vacuo