HRID728017

反应详情

EQUATION

反应方程式

HRID 728017 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A stirred mixture of 4,5-diamino-2-(2-propoxyphenyl)pyrimidin-6-one sulphate (1.0 g), triethylamine (0.42 ml) and diethyl oxalate (1.2 ml) in methoxyethanol (10 ml) was heated under reflux for 7 hours. The reaction mixture was stirred overnight at ambient temperature and a precipitate was collected and washed with water and ethanol to afford a crude product (0.70 g, m.p. 312°-315° C.). The crude product together with another sample (0.34 g) similarly prepared was twice recrystallised from dimethylformamide to afford the title compound, 0.40 g, m.p. 320°-321° C.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 7 hours
  3. customa precipitate was collected
  4. washwashed with water and ethanol
  5. customto afford a crude product (0.70 g, m.p. 312°-315° C.)
  6. customwas twice recrystallised from dimethylformamide