HRID1260631

反应详情

EQUATION

反应方程式

HRID 1260631 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A cooled (0° C.), stirred suspension of (2-chloro-4-methanesulfonyl-phenyl)-methanol (19.1 g, 0.087 mol) in diethyl ether (250 ml) under an inert atmosphere, is treated with phosphorus tribromide (5.2 ml, 0.029 mol) and allowed to stir and warm to room temperature overnight. The resulting mixture is diluted with water (100 ml) and the organic portion is separated and dried over NaOH pellets for 5 minutes. The solvent is removed in vacuo and the resulting crude residue is loaded on a pre-packed Isolute™ silica column and eluted with iso-hexane/ethyl acetate (4:1) to yield the titled compound as a white powder.

WORKUP

后处理

  1. stirringto stir
  2. temperaturewarm to room temperature overnight
  3. customthe organic portion is separated
  4. dry with materialdried over NaOH pellets for 5 minutes
  5. customThe solvent is removed in vacuo
  6. washeluted with iso-hexane/ethyl acetate (4:1)