HRID621719
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
- 20 °C
PROCEDURE
实验过程
38 g of sodium hypochlorite solution (prepared by passing about 18 g of chlorine into 220 g of 20% strength sodium hydroxide solution) are added dropwise to 13.5 (0.04 mol) of N-(2,3,6-trichloro-4-trifluoromethylphenyl)-N'-2-cyano-ethylhydrazine in 80 ml of ethanol at 10° C. The mixture is stirred at 20° C. for 16 hours, 0.5 g of solid sodium hydroxide are added and the mixture is subsequently stirred for 6 hours. It is concentrated, the residue is taken up in methylene chloride, the mixture is washed twice with water and concentrated and the residue is distilled. 10 g (76% of theory) of 1-(2,3,6-trichloro-4-trifluoromethylphenyl)-5-amino-pyrazole are obtained.
WORKUP
后处理
- stirringthe mixture is subsequently stirred for 6 hours
- concentrationIt is concentrated
- washthe mixture is washed twice with water
- concentrationconcentrated
- distillationthe residue is distilled