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
- 60 °C
PROCEDURE
实验过程
A mixture 3(2,2-dichlorovinyloxy)benzyl bromide (2.8 g), sodium p-toluene sulphonate (2.0 g) and methanol (20 ml) is warmed to 50° C for 1 hour, after which water (20 ml) and toluene (20 ml) is added with agitation. The toluene layer is separated, washed with water and concentrated by evaporation of the solvent under reduced pressure. The concentrate is then added dropwise to a 15% (w/v) aqueous solution of potassium hydroxide (100 ml) and the mixture warmed to 60° C for 1 hour, cooled to the ambient temperature and extracted with a mixture of toluene (10 ml) and methyl iso-butylketone (10 ml), the extracts dried over anhydrous magnesium sulphate and the solvents evaporated under reduced pressure to yield 3(2,2-dichlorovinyloxy)benzyl alcohol as a residual pale yellow oil.
WORKUP
后处理
- customThe toluene layer is separated
- washwashed with water
- concentrationconcentrated by evaporation of the solvent under reduced pressure
- additionThe concentrate is then added dropwise to a 15% (w/v) aqueous solution of potassium hydroxide (100 ml)
- temperaturecooled to the ambient temperature
- extractionextracted with a mixture of toluene (10 ml) and methyl iso-butylketone (10 ml)
- dry with materialthe extracts dried over anhydrous magnesium sulphate
- customthe solvents evaporated under reduced pressure