HRID358402

反应详情

EQUATION

反应方程式

HRID 358402 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
135 °C

PROCEDURE

实验过程

108 g (1 mol) of phenyl hydrazine and 60 g (1 mol) of urea were suspended in 500 ml of xylene and 111 g (1 mol) of concentrated sulfuric acid were added while stirring vigorously. The mixture was heated for 2.5 hours at 135° C. and water formed was separated via a water separator. After cooling to 90° C. 135.2 g (2.5 mols) of 85% formic acid and 25 g (0.25 mol) of concentrated sulfuric acid were added successively and the mixture was further heated for 6 hours at 95° C. After cooling, the product was filtered off, washed thoroughly with water until free from acid and dried in vacuo at 100° C. There were obtained 124.6 g (77.5% of the theory) of 1-phenyl-3-hydroxy-1,2,4-triazole having a melting point of 281°-282° C.

WORKUP

后处理

  1. customwas separated via a water separator
  2. temperatureAfter cooling to 90° C
  3. temperaturethe mixture was further heated for 6 hours at 95° C
  4. temperatureAfter cooling
  5. filtrationthe product was filtered off
  6. washwashed thoroughly with water until free from acid
  7. customdried in vacuo at 100° C