HRID1721921

反应详情

EQUATION

反应方程式

HRID 1721921 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

12.7 parts of the 2-(4'-chloro-2'-difluoromethoxyphenyl)-2-methyl-4-ethyl-1,3-dioxolane prepared in (a) are dissolved in 100 ml of abs. chloroform and the solution is warmed to 30° C. Under irradiation with a 150 watt spot lamp, 7.3 parts of bromine in 30 ml of abs. chloroform are added dropwise over 1 hour and the reaction mixture is then stirred for 2 hours at room temperature. The reaction mixture is then washed with 2×100 ml of water, dried over sodium sulfate, and filtered. The solvent is removed by evaporation and the oily residue is purified by high vacuum distillation; b.p. 113°-115° C./0.05 mbar.

WORKUP

后处理

  1. dissolutionare dissolved in 100 ml of abs
  2. washThe reaction mixture is then washed with 2×100 ml of water
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. customThe solvent is removed by evaporation
  6. distillationthe oily residue is purified by high vacuum distillation