HRID1288283

反应详情

EQUATION

反应方程式

HRID 1288283 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A cold solution of benzenediazonium chloride [prepared, by the method well known in the art, from 13.3 g. aniline in a 1:1 v/v mixture of water and concentrated hydrochloric acid (120 ml)] was added dropwise with stirring to a solution of 4-amino-2-isopropylpyrimid-6-one (28 g.) and sodium hydroxide (14.8 g.) in water (450 ml.) at 5° C. After stirring for a further 1 hour, the mixture was filtered. The filtrate was adjusted to pH 6 by the addition of aqueous sodium hydroxide solution, and the resultant solid was isolated to give crude 4-amino-2-isopropyl-5-phenylazopyrimid-6-one (33.5 g.), m.p. 215°-219° C. Recrystallisation from ethanol gave pure 4-amino-2-isopropyl-5-phenylazopyrimid-6-one (8.3 g.), m.p. 235°-236° C. (with decomposition).

WORKUP

后处理

  1. additionwas added dropwise
  2. filtrationthe mixture was filtered
  3. additionThe filtrate was adjusted to pH 6 by the addition of aqueous sodium hydroxide solution
  4. customthe resultant solid was isolated
  5. customto give crude 4-amino-2-isopropyl-5-phenylazopyrimid-6-one (33.5 g.), m.p. 215°-219° C
  6. customRecrystallisation from ethanol