HRID1288279

反应详情

EQUATION

反应方程式

HRID 1288279 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Sodium dithionite (30 g.) was added in portions to an agitated suspension of 4-amino-2-benzyl-5-phenylazo-pyrimid-6-one (14 g.) in a mixture of ethanol (200 ml.) and 2N aqueous sodium hydroxide solution (200 ml.) maintained at a temperature near to the reflux temperature. The mixture was then heated under reflux for 20 minutes, treated with a further quantity of sodium dithionite (20 g.) and the mixture heated under reflux for a further 30 minutes. The mixture was then evaporated to dryness, the residue was dissolved in water (200 ml.), acidified to pH 6 by means of concentrated hydrochloric acid, cooled to 0° C, and filtered. The solid thus obtained was recrystallised from water to give 4,5-diamino-2-benzyl-pyrimid-6-one (4.4 g.), m.p. 243°-246° C.

WORKUP

后处理

  1. temperaturemaintained at a temperature near to the reflux temperature
  2. temperatureThe mixture was then heated
  3. temperatureunder reflux for 20 minutes
  4. temperaturethe mixture heated
  5. temperatureunder reflux for a further 30 minutes
  6. customThe mixture was then evaporated to dryness
  7. dissolutionthe residue was dissolved in water (200 ml.)
  8. filtrationfiltered
  9. customThe solid thus obtained
  10. customwas recrystallised from water