Sodium Hydroxide → HCID 178526413, Verbindung

HRID 1031113Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1031113
[OH:1][C:2]1[C:3]([OH:16])=[N:4][C:5]2[C:6]([N:15]=1)=[C:7]1[C:12](=[CH:13][CH:14]=2)[N:11]=[CH:10][CH:9]=[N:8]1.[N+:17]([O-])([O-:19])=[O:18].[K+].[OH-].[Na+]>S(=O)(=O)(O)O>[OH:1][C:2]1[C:3]([OH:16])=[N:4][C:5]2[C:6]([N:15]=1)=[C:7]1[C:12](=[C:13]([N+:17]([O-:19])=[O:18])[CH:14]=2)[N:11]=[CH:10][CH:9]=[N:8]1

Komponenten

5

Edukt 3

HCID 14798Sodium HydroxideHCID 24434Potassium NitrateHCID 178516995HCID 178516995, Verbindung

Produkt 1

HCID 178526413HCID 178526413, VerbindungAusbeute 47 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1118Sulfuric AcidLösungsmittel

Versuchsvorschrift

To a solution of 0,38 g (1,4 mmol) 2,3-dihydroxy-pyrazino(2,3-f)quinoxaline in 25 ml concentrated sulfuric acid was added at 0° C. 0,28 g (2,8 mmol) potassium nitrate. Stirring was continued at 0° C. for 30 min. and at 25° C. for 24 h. The reaction mixture was poured into 100 ml ice-water. The solution was added 10N sodium hydroxide to pH 7, and then extracted with ethyl acetate (5×100 ml). The combined and dried ethyl acetate phases were evaporated to give 0,17 g (47%) 2,3-dihydroxy-6-nitropyrazino(2,3-f)quinoxaline, m.p. >300° C. NMR (DMSO-d6): 9.10 (2H,s), 8.23 (1H,s).

Aufarbeitung

  1. extractionextracted with ethyl acetate (5×100 ml)
  2. customdried ethyl acetate phases were evaporated

Quellen und Nachweise

ORD-Eintrag
ord-0005ecd356ed498788020d03adca5d07
Quelldatensatz
uspto-grants-1992_04
Patentnummer
US05109001

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