反应详情

Heat a solution of 2-(4-fluoro-2-nitro-phenylamino)-5-trifluoromethyl-benzonitrile (9.995 g, 30.73 mmol) in ethanol (170 ml) to 60° C. Add to this a solution of tin (II) chloride (29.1 g, 153.67 mmol) in 5.0 N hydrochloric acid (170 ml). Heat the resulting mixture to reflux for 18 hours. Cool the reaction to room temperature and place in a freezer for 24 hours. Precipitate the product from the solution and collect by filtration to btain 2.253 g of the title compound (6.79 mmol, 22% yield) as a yellow amorphous solid: Mass Spectrum (m/e): 296(M+1).

1. temperatureHeat the resulting mixture
2. temperatureto reflux for 18 hours
3. temperatureCool
4. customthe reaction to room temperature
5. filtrationPrecipitate the product from the solution and collect by filtration