HRID263047

反应详情

EQUATION

反应方程式

HRID 263047 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a stirred solution of 120 parts of 1-(2,3-dichlorophenyl)-1-ethanone in 240 parts of butanol are added dropwise 101 parts of bromine at room temperature. After stirring for 1 hour at room temperature, there are added successively 42 parts of 1,2-ethanediol, 540 parts of anhydrous benzene and 4 parts of 4-methylbenzenesulfonic acid. The whole is stirred and refluxed overnight with water-separator. The reaction mixture is evaporated and the residue is dissolved in 2,2'-oxybispropane. The solution is washed with a diluted sodium hydroxide solution and three times with water, dried, filtered and evaporated. The residue is distilled, yielding 96.6 parts (49%) of 2-(bromomethyl)-2-(2,3-dichlorophenyl)-1,3-dioxolane; bp. 135°-137° C. at 0.1 mm. pressure.

WORKUP

后处理

  1. stirringThe whole is stirred
  2. customThe reaction mixture is evaporated
  3. dissolutionthe residue is dissolved in 2,2'-oxybispropane
  4. washThe solution is washed with a diluted sodium hydroxide solution and three times with water
  5. customdried
  6. filtrationfiltered
  7. customevaporated
  8. distillationThe residue is distilled