Water → 6-Ethyl-2-oxo-1-phenyl-1,2-dihydropyridine-3-carboxylic acid
Reaktionsgleichung
[CH2:1]([C:3]1[N:8]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[C:7](=[O:15])[C:6]([C:16]#N)=[CH:5][CH:4]=1)[CH3:2].[OH-:18].[Na+].[OH2:20]>S(=O)(=O)(O)O>[CH2:1]([C:3]1[N:8]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[C:7](=[O:15])[C:6]([C:16]([OH:20])=[O:18])=[CH:5][CH:4]=1)[CH3:2]Komponenten
5
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 120 °C
Versuchsvorschrift
6-Ethyl-2-oxo-1-phenyl-1,2-dihydropyridine-3-carbonitrile (395 mg, 1.76 mmol) was dissolved in conc. sulfuric acid (0.4 mL) and water (0.4 mL), and the mixture was stirred with heating at 120° C. for 7 hr. 1N Aqueous sodium hydroxide solution was added to the reaction solution, and the mixture was washed with ethyl acetate. 1N Hydrochloric acid was added to the aqueous layer, and the mixture was extracted 3 times with ethyl acetate. The combined organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate and filtered, and the solvent was evaporated under reduced pressure. The residue was washed with ethyl acetate to give the title compound (310 mg, 72%) as a colorless solid.
Aufarbeitung
- washthe mixture was washed with ethyl acetate
- addition1N Hydrochloric acid was added to the aqueous layer
- extractionthe mixture was extracted 3 times with ethyl acetate
- washThe combined organic layer was washed with saturated brine
- dry with materialdried over anhydrous magnesium sulfate
- filtrationfiltered
- customthe solvent was evaporated under reduced pressure
- washThe residue was washed with ethyl acetate
Quellen und Nachweise
- ORD-Eintrag
- ord-f5dd924ee3ba496badf11f1d708f9a35
- Quelldatensatz
- uspto-grants-2013_05
- Patentnummer
- US08445509B2
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