HRID2279703

反应详情

EQUATION

反应方程式

HRID 2279703 的结构方程式

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture of 4-(chloromethyl)-2-methoxy-1-nitrobenzene (Compound 1H, 1.1 g, 5.46 mmol) and triethyl phosphite (1.09 g, 6.55 mmol) were heated at 100° C. for 16 h in a sealed tube. The reaction mixture was concentrated under reduced pressure to yield a black oil. The crude material was purified by silica gel chromatography on a Teledyne ISCO CombiFlash® Rf system using DCM/MeOH (100:0→95:5) as eluent to afford the title compound as 1.08 g of an orange oil (65%). MS (ESI): m/z 304.0902 [M+H]+.

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. customto yield a black oil
  3. customThe crude material was purified by silica gel chromatography on a Teledyne ISCO CombiFlash® Rf system