HRID1288278

反应详情

EQUATION

反应方程式

HRID 1288278 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of sodium dithionite (62 g.) in water (300 ml.) was added dropwise during 30 minutes to a solution of 4-amino-2-benzyl-5-phenylazopyrimid-6-one (27 g.) in dimethylformamide (1000 ml.) at 75° C. The mixture was cooled, and the insoluble solid was filtered off. The filtrate was evaporated in vacuo, the residue was stirred with water, and the solid filtered off. This solid was extracted with boiling water (250 ml.), the extract was filtered hot and then cooled. The solid which separated was recrystallised from water to give 4,5-diamino-2-benzylpyrimid-6-one (12.4 g.) in the form of off-white needles, m.p. 243° C. (with decomposition).

WORKUP

后处理

  1. temperatureThe mixture was cooled
  2. filtrationthe insoluble solid was filtered off
  3. customThe filtrate was evaporated in vacuo
  4. filtrationthe solid filtered off
  5. extractionThis solid was extracted with boiling water (250 ml.)
  6. filtrationthe extract was filtered hot
  7. temperaturecooled
  8. customThe solid which separated
  9. customwas recrystallised from water