HRID487889

反应详情

EQUATION

反应方程式

HRID 487889 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2,6-bis(bromomethyl)-1-fluorobenzene (2.82 g, 0.010 mole) and trimethylphosphite (5.0 mL, 0.042 mole) in toluene (25 mL) is heated at reflux temperature for 24 hours, after which the solvent and excess trimethylphosphite are removed under reduced pressure. The solid residue is crystallized from ethyl acetate-hexane, giving 3.12 g (0.0089 mole, 89%) of of the title compound, mp 116.5°-117.5° C. Recrystallization gives 2.64 g, mp 117°-118° C.

WORKUP

后处理

  1. temperatureat reflux temperature for 24 hours
  2. customafter which the solvent and excess trimethylphosphite are removed under reduced pressure
  3. customThe solid residue is crystallized from ethyl acetate-hexane