HRID274318

反应详情

EQUATION

反应方程式

HRID 274318 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

86.0 g (0.3 mol) of phosphorus oxybromide was added to 73.1 g (1.0 mol) of N,N-dimethylformamide, and 15.1 g (0.1 mol)of guanine (manufactured by Sumika Fine Chemicals Co., Ltd.) was then added, followed by stirring at 100° C. for 4 hours. After cooling, 200 ml of water was carefully added at 20° C. After stirring at room temperature for 24 hours, the precipitating crystal was collected by filtration and dissolved in 200 ml of 25% aqueous ammonia with heating, and the insoluble substances were filtered out. The mother liquor was concentrated under reduced pressure, and the precipitating crystal was collected by filtration to yield 11.1 g (0.052 mol) of a pale yellow crystal of 2-amino-6-bromopurine (yield 52%). Its properties are as follows:

WORKUP

后处理

  1. additionwas then added
  2. temperatureAfter cooling
  3. stirringAfter stirring at room temperature for 24 hours
  4. filtrationthe precipitating crystal was collected by filtration
  5. dissolutiondissolved in 200 ml of 25% aqueous ammonia
  6. temperaturewith heating
  7. filtrationthe insoluble substances were filtered out
  8. concentrationThe mother liquor was concentrated under reduced pressure
  9. filtrationthe precipitating crystal was collected by filtration