反应详情

A mixture of 3-(2,4-difluorophenylamino)-4-nitrobenzonitrile (3.5 g), iron powder (3.5 g) and ammonium chloride (0.35 g) in ethanol (50 ml) and water (25 ml) was refluxed for 1 hour. The insoluble material was filtered and the filtrate was concentrated. The residue was dissolved in ethyl acetate, washed with water, dried and evaporated to dryness. The residual oil (3 g) was purified by column chromatography on silica gel (100 g) eluting with a mixture of toluene and ethyl acetate to give a powder of 4-amino-3-(2,4-difluorophenylamino)benzonitrile (1.2 g).

1. temperaturewas refluxed for 1 hour
2. filtrationThe insoluble material was filtered
3. concentrationthe filtrate was concentrated
4. dissolutionThe residue was dissolved in ethyl acetate
5. washwashed with water
6. customdried
7. customevaporated to dryness
8. customThe residual oil (3 g) was purified by column chromatography on silica gel (100 g)
9. washeluting with a mixture of toluene and ethyl acetate