Reaktion #70862

Reaktionsgleichung

Water

EtOAc

KOH

4,6-bis(4-fluorophenyl)-5-(4-pyridyl)-1H-pyrazolo[3,4-b]pyridine-3-carbonitrile

4,6-Bis(4-fluorophenyl)-5-(4-pyridyl)-1H-pyrazolo[3,4-b]pyridine-3-carbonitrile

→

title compound

Ausbeute 28.0%

4,6-Bis(4-fluorophenyl)-5-(4-pyridyl)-1H-pyrazolo[3,4-b]pyridine-3-carboxamide

Ausbeute 28.0%

Lösungsmittel

tBuOH

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturheated
2. 2
   Temperaturto reflux overnight
3. 3
   Sonstigethe phases were separated
4. 4
   ExtraktionThe aqueous phase was extracted with EtOAc
5. 5
   TrocknenThe combined organic phases were dried over Na2SO4
6. 6
   Einengenconcentrated to dryness
7. 7
   SonstigeThe crude product obtained
8. 8
   Sonstigewas purified by chromatography on silica gel
9. 9
   Temperaturof increasing polarity as eluent

Vorschrift

A solution of KOH (0.07 g, 1.3 mmol) in tBuOH (2.5 mL) was added under argon atmosphere to 4,6-bis(4-fluorophenyl)-5-(4-pyridyl)-1H-pyrazolo[3,4-b]pyridine-3-carbonitrile (0.05 g, 0.1 mmol, obtained in example 65) and heated to reflux overnight. Water and EtOAc were added and the phases were separated. The aqueous phase 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 15 mg of the title compound in solid form (yield: 28%)

Quelle