HRID131331

反应详情

EQUATION

反应方程式

HRID 131331 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-(5-fluoro-2-nitro-phenylamino)-5-isopropyl-benzonitrile (0.372 g, 1.24 mmol) in ethanol (6 ml) to 60° C. Add a solution of tin (II) chloride (0.707 g, 3.73 mmol) in 5.0 N hydrochloric acid (6 ml) and heat the resulting mixture to reflux for 16 hours. Cool the reaction to room temperature, add 30 ml of 5.0 N hydrochloric acid and place the mixture in a freezer for 16 hours. Precipitate the product from the solution and collect by filtration. Wash solid with 5.0 N hydrochloric acid to obtain 0.365 g of the title compound (1.19 mmol, 96% yield) as a yellow amorphous solid: Mass Spectrum (m/e): 270(M+1).

WORKUP

后处理

  1. temperatureheat the resulting mixture
  2. temperatureto reflux for 16 hours
  3. temperatureCool
  4. customthe reaction to room temperature
  5. filtrationPrecipitate the product from the solution and collect by filtration
  6. washWash solid with 5.0 N hydrochloric acid