HRID846877

反应详情

EQUATION

反应方程式

HRID 846877 的结构方程式

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

55 ml (0.46 mol) of tin tetrachloride are added dropwise with cooling in an ice bath (exothermic reaction) to a solution of 230 ml (2.43 mol) of chloromethyl ethyl ether and 197 g (1.22 mol) of 1,3-diisopropylbenzene in 600 ml of carbon tetrachloride and the mixture is stirred at 0° C. for 1 h. After stirring overnight at +25° C., 142 g (1.5 mol) of chloromethyl ethyl ether and 74 ml (0.46 mol) of tin tetrachloride are again added dropwise at 0° C. and the mixture is stirred overnight at +25° C. The reaction mixture is added to ice/hydrochloric acid, and the organic phase is separated off, washed with water and dried using sodium sulphate. After concentrating, the residue is taken up with petroleum ether, filtered through 1 kg of silica gel (230-400 mesh) and distilled in a high vacuum.

WORKUP

后处理

  1. temperaturewith cooling in an ice bath
  2. stirringAfter stirring overnight at +25° C.
  3. stirringthe mixture is stirred overnight at +25° C
  4. customthe organic phase is separated off
  5. washwashed with water
  6. customdried
  7. concentrationAfter concentrating
  8. filtrationfiltered through 1 kg of silica gel (230-400 mesh)
  9. distillationdistilled in a high vacuum