反应详情

温度

200 °C

A mixture of 3-chloro-4-nitrobenzonitrile (5 g), 2,4-difluoroaniline (17.7 g), cupric oxide (0.5 g) and potassium carbonate (4.5 g) was stirred for 5 hours at 200° C. To the mixture were added water (100 ml) and ethyl acetate (200 ml). The organic layer was separated, washed with 3N hydrochloric acid and water, dried, and evaporated to dryness. The oil (10 g) was purified by column chromatography on silica gel (200 g) eluting with toluene to give red crystals of 3-(2,4-difluorophenylamino)-4-nitrobenzonitrile (3.5 g).

1. customThe organic layer was separated
2. washwashed with 3N hydrochloric acid and water
3. customdried
4. customevaporated to dryness
5. customThe oil (10 g) was purified by column chromatography on silica gel (200 g)
6. washeluting with toluene