HRID372472

反应详情

EQUATION

反应方程式

HRID 372472 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

A mixture of 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

  1. customThe toluene layer is separated
  2. washwashed with water
  3. concentrationconcentrated by evaporation of the solvent under reduced pressure
  4. additionThe concentrate is then added dropwise to a 15% (w/v) aqueous solution of potassium hydroxide (100 ml)
  5. temperaturethe mixture warmed to 60° C for 1 hour
  6. temperaturecooled to the ambient temperature
  7. extractionextracted with a mixture of toluene (10 ml) and methyl iso-butylketone (10 ml)
  8. dry with materialthe extracts dried over anhydrous magnesium sulphate
  9. customthe solvents evaporated under reduced pressure