Reaktion #595356
ord-963d645643a140edb98468049189ceca
Reaktionsgleichung
compound
2-Amino-4-[4-(2-hydroxyethoxy)phenyl]-6-(phenylsulfanyl)pyridine-3,5-dicarbonitrile
sodium hydroxide
→
6-Amino-4-[4-(2-hydroxyethoxy)phenyl]-2-oxo-1,2-dihydropyridine-3,5-dicarbonitrile
Edukte
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Temperatur
80°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Sonstigea clear solution is formed
- 2TemperaturAfter cooling to RT
- 3Sonstigethe solvent is removed on a rotary evaporator
- 4Sonstigeis formed
- 5workup.STIRRINGThe suspension is stirred at RT for 3 h
- 6FiltrationThe precipitate is filtered off
- 7Waschenwashed with about 5 ml of water
- 8Sonstigea little ethanol and then recrystallized from about 10 ml of ethanol
- 9SonstigeThe product obtained in this manner
- 10Sonstigeis used without further purification in the subsequent reactions
Vorschrift
500 mg (1.29 mmol) of the compound from Example 99A are initially charged in 6.4 ml of ethanol. After addition of 2.57 g (28.96 mmol) of sodium hydroxide, the mixture is stirred at 80° C. for 30 min, and a clear solution is formed. After cooling to RT, the solvent is removed on a rotary evaporator. The residue is taken up in 3 ml of water and acidified with 1 N hydrochloric acid until a yellowish precipitate is formed. The suspension is stirred at RT for 3 h. The precipitate is filtered off, washed with about 5 ml of water and a little ethanol and then recrystallized from about 10 ml of ethanol. The product obtained in this manner is used without further purification in the subsequent reactions.