反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customwas separated via a water separator
- temperatureAfter cooling to 90° C
- temperaturethe mixture was further heated for 6 hours at 95° C
- temperatureAfter cooling
- filtrationthe product was filtered off
- washwashed thoroughly with water until free from acid
- customdried in vacuo at 100° C