HRID1669526

反应详情

EQUATION

反应方程式

HRID 1669526 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a solution of 2-(4-Phenoxy-phenoxy)-ethanol (2.2 g, 9.55 mmol), triphenylphosphine (2.76 g, 10.5 mmol), and dichloromethane (DCM) (36.7 mL) after stirring at 0° C., was added N-Bromosuccinimide (1.87 g, 10.5 mmol). The resulting mixture was stirred at 0° C. for 30 minutes and then at room temperature for 30 minutes. Reaction mixture was concentrated in vacuo to obtain the crude mixture, which was purified by of silica gel flash chromatography, using EtOAc/hexane (gradient system), to obtain the product (2.5 g, 89%): 1H NMR (400 MHz, CDCL3).

WORKUP

后处理

  1. waitat room temperature for 30 minutes
  2. customReaction mixture
  3. concentrationwas concentrated in vacuo
  4. customto obtain the crude mixture, which
  5. customwas purified by of silica gel flash chromatography