反应详情

0.74 g of 4-bromo-2-fluorobenzonitrile, 3.07 g of caesium carbonate, 0.172 g of (9,9-dimethyl-9H-xanthene-4,5-diyl)bis(diphenylphosphane) and 0.055 g of palladium acetate are successively added, under argon, to a solution of 0.68 g of 4-(5-methoxypyridin-3-yl)-9H-carbazole in 30 ml of dioxane. The reaction mixture is refluxed for 2 and a half hours, cooled to ambient temperature, filtered through celite and concentrated under reduced pressure. The residue is purified by silica gel chromatography, elution being carried out with a mixture of cyclohexane and ethyl acetate (80/20 by volume), so as to give 0.78 g of 2-fluoro-4-[4-(5-methoxypyridin-3-yl)-9H-carbazol-9-yl]benzonitrile in the form of a colourless oil, the characteristics of which are the following:

1. temperatureThe reaction mixture is refluxed for 2 and a half hours
2. filtrationfiltered through celite and
3. concentrationconcentrated under reduced pressure
4. customThe residue is purified by silica gel chromatography, elution
5. additionbeing carried out with a mixture of cyclohexane and ethyl acetate (80/20 by volume)