HRID1075447

反应详情

EQUATION

反应方程式

HRID 1075447 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of 4-fluoro-3-nitroaniline (20g, 0.13mol) in toluene (200mi) is added 2,5-dimethoxytetrahydrofuran (33ml, 0.26mol) and a catalytic amount of pTSA. The mixture is refluxed for 2.5 hours. After cooling the solvent is removed by evaporation and the residue is purified by column chromatography on silica gel using a mixture of ethyl acetate and petroleum ether (1:1) as the eluent. Yield: 23.1g (87%). Mp 79-81° C.

WORKUP

后处理

  1. temperatureThe mixture is refluxed for 2.5 hours
  2. temperatureAfter cooling the solvent
  3. customis removed by evaporation
  4. customthe residue is purified by column chromatography on silica gel using
  5. additiona mixture of ethyl acetate and petroleum ether (1:1) as the eluent