Potassium Carbonate → HCID 117770718, Verbindung

HRID 1526387

Reaktionsgleichung

[CH3:1][O:2][C:3]1[CH:8]=[CH:7][NH:6][C:5](=[O:9])[C:4]=1[C:10]#[N:11].[F:12][C:13]1[CH:14]=[C:15]([CH:18]=[C:19]([F:22])[C:20]=1F)[C:16]#[N:17].C(=O)([O-])[O-].[K+].[K+].C(=O)([O-])O.[Na+]>CN(C)C=O>[C:16]([C:15]1[CH:14]=[C:13]([F:12])[C:20]([N:6]2[CH:7]=[CH:8][C:3]([O:2][CH3:1])=[C:4]([C:10]#[N:11])[C:5]2=[O:9])=[C:19]([F:22])[CH:18]=1)#[N:17]

Komponenten

Reaktionsbedingungen

Temperatur: 50 °C

Versuchsvorschrift

A mixture of 4-methoxy-2-oxo-1,2-dihydropyridine-3-carbonitrile (2.00 g), 3,4,5-trifluorobenzonitrile (2.93 g), potassium carbonate (3.68 g) and N,N-dimethylformamide (20 mL) was stirred at 50° C. for 5 hr. The reaction mixture was slowly poured into saturated sodium hydrogen carbonate solution, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. To the residue was added a mixed solvent (10 mL) of isopropyl ether/ethyl acetate=4/1, and the mixture was stirred for 15 min. The precipitate was collected by filtration to give the title compound (1.65 g).

Aufarbeitung

extractionthe mixture was extracted with ethyl acetate
washThe extract was washed with saturated brine
dry with materialdried over anhydrous magnesium sulfate
customthe solvent was evaporated under reduced pressure
additionTo the residue was added a mixed solvent (10 mL) of isopropyl ether/ethyl acetate=4/1
stirringthe mixture was stirred for 15 min
filtrationThe precipitate was collected by filtration

Quellen und Nachweise

ORD-Eintrag: ord-4a47bf8505ac4472bc43a66e5f332700
Quelldatensatz: uspto-grants-2015_07
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US09085578B2

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