HRID131321

反应详情

EQUATION

反应方程式

HRID 131321 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Heat a solution of 2-(4-fluoro-2-nitro-phenylamino)-5-methyl-benzonitrile (1.747 g, 6.44 mmol) in ethanol (35 ml) to 60° C. Add a solution of tin (II) chloride (6.06 g, 31.96 mmol) in 5.0 N hydrochloric acid (35 ml) and heat the resulting mixture to reflux for 40 hours. Cool the reaction to room temperature and place in a freezer for 16 hours. Collect by filtration the product precipitates from the solution to obtain 1.3 g of the title compound (4.68 mmol, 73% yield) as a yellow-green amorphous solid: Mass Spectrum (m/e): 241(M+1).

WORKUP

后处理

  1. temperatureheat the resulting mixture
  2. temperatureto reflux for 40 hours
  3. temperatureCool
  4. customthe reaction to room temperature
  5. filtrationCollect by filtration the product
  6. customprecipitates from the solution