反应详情

In a volumetric flask, 3-bromo-4,6-bis(4-fluorophenyl)-5-(4-pyridyl)-1H-pyrazolo[3,4-b]pyridine (0.20 g, 0.4 mmol, obtained in example 64), copper cyanide (I) (0.05 g, 0.6 mmol) and anhydrous 1-methyl-2-pyrrolidone (1 mL) were introduced under argon atmosphere and heated to reflux for 2 h. This was poured into a 10% aqueous solution of ethylendiamine (4 mL) and extracted with CHCl3. Brine was added to the aqueous phase and it was extracted with EtOAc. The combined organic phases were dried over Na2SO4 and concentrated to dryness. The crude product obtained was purified by chromatography on silica gel using hexane-EtOAc mixtures of increasing polarity as eluent, to afford the title compound in a solid form (yield: quantitative).

1. temperatureheated
2. temperatureto reflux for 2 h
3. extractionextracted with CHCl3
4. additionBrine was added to the aqueous phase and it
5. extractionwas extracted with EtOAc
6. dry with materialThe combined organic phases were dried over Na2SO4
7. concentrationconcentrated to dryness
8. customThe crude product obtained
9. customwas purified by chromatography on silica gel
10. temperatureof increasing polarity as eluent