HRID743380

反应详情

EQUATION

反应方程式

HRID 743380 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

16.4 ml of carbon tetrachloride, followed by 44.5 g of triphenylphosphine were added, whilst ice-cooling, to a solution of 23.8 g of 2-methoxymethoxybenzyl alcohol in 240 ml of tetrahydrofuran, and the resulting mixture was heated under reflux for 5 hours. At the end of this time, the mixture was cooled, insoluble materials were filtered off and the filtrate was concentrated by evaporation under reduced pressure. The resulting residue was purified by column chromatography through silica gel, using a 9:1 by volume mixture of hexane and ethyl acetate as the eluent, to give 15.5 g (yield 57%) of the title compound as a colorless liquid.

WORKUP

后处理

  1. additionwere added, whilst ice-
  2. temperaturethe resulting mixture was heated
  3. temperatureunder reflux for 5 hours
  4. temperatureAt the end of this time, the mixture was cooled
  5. filtrationinsoluble materials were filtered off
  6. concentrationthe filtrate was concentrated by evaporation under reduced pressure
  7. customThe resulting residue was purified by column chromatography through silica gel
  8. additionby volume mixture of hexane and ethyl acetate as the eluent