反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
28.45 g (0.1 mol) of 1-(4-chlorophenoxy)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)-butan-2-one and 43.25 g (0.1 mol) of formic acid/triethylamine (5:2 addition compound) were heated to 145° to 150° C. for 4.5 to 5 hours. The reaction mixture was allowed to cool and was concentrated in vacuo. The residue was taken up in dilute sodium hydroxide solution and the mixture was extracted with methylene chloride. The organic phase was washed with water, dried over sodium sulphate and concentrated in vacuo. The residue was suspended in hot cyclohexane, the suspension was filtered hot and the solid was dried. 18.2 g (63.6% of theory) of 1-(4-chlorophenoxy)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)-butan-2-ol of melting point 114°-116° C. were obtained.
WORKUP
后处理
- temperatureto cool
- concentrationwas concentrated in vacuo
- extractionthe mixture was extracted with methylene chloride
- washThe organic phase was washed with water
- dry with materialdried over sodium sulphate
- concentrationconcentrated in vacuo
- filtrationthe suspension was filtered hot
- customthe solid was dried