Dimethyl Sulfoxide → HCID 22903580, Verbindung

HRID 1488970

Reaktionsgleichung

Reaktionsgleichung von HRID 1488970
F[C:2]1[CH:11]=[C:10]2[C:5]([NH:6][C:7](=[O:13])[C:8](=[O:12])[NH:9]2)=[CH:4][C:3]=1[N+:14]([O-:16])=[O:15].[Cl:17][C:18]1[CH:19]=[N:20][CH:21]=[C:22]([Cl:25])[C:23]=1[OH:24].[OH-].[K+].CS(C)=O>CC(C)=O>[N+:14]([C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:2]=1[N:20]1[CH:21]=[C:22]([Cl:25])[C:23](=[O:24])[C:18]([Cl:17])=[CH:19]1)[NH:9][C:8](=[O:12])[C:7](=[O:13])[NH:6]2)([O-:16])=[O:15]

Komponenten

6

Edukt 4

HCID 679Dimethyl SulfoxideHCID 14797Potassium HydroxideHCID 99912306-Fluoro-7-nitro-1,4-dihydroquinoxaline-2,3-dioneHCID 178516337HCID 178516337, Verbindung

Produkt 1

HCID 22903580HCID 22903580, VerbindungAusbeute 79,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel

Versuchsvorschrift

First, 1.129 g of 7-fluoro-6-nitro-1,4-dihydroquinoxaline-2,3-dione, 1.648 g of 3,5-dichloro-4-hydroxypyridine, and 672 mg of powdered potassium hydroxide were added to 10 ml of dry dimethylsulfoxide. The mixture was allowed to react at 130° C. for 3 hours in a nitrogen atmosphere. The subsequent processes were conducted in the same way as in Example 2. The resultant precipitate was dissolved by heating in dimethylformaldehyde and the solution was decolorized with activated carbon and filtered. Water in an equal amount was added thereto and the solution was allowed to stand overnight to give 1.473 g of crystals of 6-nitro-7-(3,5-dichloro-4-oxo-4H-pyridin-1-yl)-1,4-dihydroquinoxaline-2,3-dione.

Aufarbeitung

  1. customto react at 130° C. for 3 hours in a nitrogen atmosphere
  2. filtrationfiltered
  3. additionWater in an equal amount was added

Quellen und Nachweise

ORD-Eintrag
ord-b1eda07ea62c4b62b01ad54716b65a27
Quelldatensatz
uspto-grants-1997_10
Patentnummer
US05677305

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