HRID2242043

反应详情

EQUATION

反应方程式

HRID 2242043 的结构方程式

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 3-trifluoromethoxy nitrobenzene (4.0 g, 20 mmol) in DMSO (60 ml), trimethylhydrazinium iodide (4.4 g, 22 mmol) is added and cooled to 0° C. KOt-Bu is added in portions. After stirring for 4 h at 25° C., ice water is added, pH is adjusted to 2-3 with HCl solution, the mixture extracted with EtOAc and washed with brine, followed by drying (Na2SO4) and evaporation of the solvent. Chromatography (silica gel, CH2Cl2/hexane=1:1) gave 2-nitro-6-trifluoromethoxy-phenylamine.

WORKUP

后处理

  1. extractionthe mixture extracted with EtOAc
  2. washwashed with brine
  3. customby drying
  4. custom(Na2SO4) and evaporation of the solvent