HRID1921868

反应详情

EQUATION

反应方程式

HRID 1921868 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4.60 g (17 mmol) of 2-(2-chlorobenzyloxy)-5-fluorobenzyl alcohol are dissolved in 10 ml of acetonitrile, then 5.62 g (16 mmol) of triphenylphosphine hydrobromide are added, and the suspension is stirred under reflux for 12 h. A further 2.80 g (8 mmol) of triphenylphosphine hydrobromide are added, and the mixture is stirred under reflux for a further 3 h. The solvent is mostly distilled out in vacuo, the crystals which have separated out are stirred with petroleum ether, filtered off with suction and dried on a clay dish. 9.82 g (15.7 mmol, 92% of theory) of the title compound are obtained.

WORKUP

后处理

  1. temperatureunder reflux for 12 h
  2. stirringthe mixture is stirred
  3. temperatureunder reflux for a further 3 h
  4. distillationThe solvent is mostly distilled out in vacuo
  5. customthe crystals which have separated out
  6. stirringare stirred with petroleum ether
  7. filtrationfiltered off with suction
  8. customdried on a clay dish