Dimethylformamide → HCID 20563052, Verbindung

HRID 127354

Reaktionsgleichung

Reaktionsgleichung von HRID 127354
N[C:2]1[O:3][C:4]2[CH:14]=[CH:13][CH:12]=[CH:11][C:5]=2[C:6](=[O:10])[C:7]=1C=O.[C:15]([C:17]#[CH:18])#[N:16].[CH3:19][N:20](C)C=O>>[C:15]([C:17]1[CH:19]=[N:20][C:7]2[C:6](=[O:10])[C:5]3[C:4]([O:3][C:2]=2[CH:18]=1)=[CH:14][CH:13]=[CH:12][CH:11]=3)#[N:16]

Komponenten

4

Edukt 3

HCID 6228DimethylformamideHCID 140552-PropynenitrileHCID 7359282-Amino-3-formylchromone

Produkt 1

HCID 20563052HCID 20563052, Verbindung

Reaktionsbedingungen

Temperatur
140 °C

Versuchsvorschrift

To 70 ml of dimethylformamide was added 2.2 g of 2-amino-4-oxo-4H-1-benzopyran-3-carboxaldehyde, followed by the addition of 2.5 g of cyanoacetylene. The mixture was heated under stirring at 140° C. for 15 hours and the solvent was then distilled off under reduced pressure. The residue was chromatographed on silica gel and eluted with chloroform and recrystallized from acetonitrile to give 0.83 g of 3-cyano-1-azaxanthone as crystals, m.p. 220°-226° C.

Aufarbeitung

  1. temperatureThe mixture was heated
  2. distillationthe solvent was then distilled off under reduced pressure
  3. customThe residue was chromatographed on silica gel
  4. washeluted with chloroform
  5. customrecrystallized from acetonitrile

Quellen und Nachweise

ORD-Eintrag
ord-1024b56898ab4dc3a52291c2bd63f8af
Quelldatensatz
uspto-grants-1981_03
Patentnummer
US04255576

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