Oxalic Acid → Pyrido(2,3-b)pyrazine-2,3-diol

HRID 655622Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 655622
[NH2:1][C:2]1[C:7]([NH2:8])=[CH:6][CH:5]=[CH:4][N:3]=1.[C:9](O)(=[O:13])[C:10](O)=[O:11]>Cl>[NH:8]1[C:10](=[O:11])[C:9](=[O:13])[NH:1][C:2]2[N:3]=[CH:4][CH:5]=[CH:6][C:7]1=2

Komponenten

4

Edukt 2

HCID 971Oxalic AcidHCID 99562,3-Diaminopyridine

Produkt 1

HCID 74947Pyrido(2,3-b)pyrazine-2,3-diolAusbeute 90,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 313Hydrochloric AcidLösungsmittel

Versuchsvorschrift

To a suspension of 2,3-diaminopyridine (20 g, 0.136 mol) in 4N aqueous HCl (200 ml) is added oxalic acid (20.7 g, 0.164 mol) and the reaction mixture is refluxed for 20 h. The reaction mixture is cooled and the solid precipitated is filtered, washed with water and dried under vacuum to afford 20 g (89%) of the title compound as a solid. HPLC (max plot) 98%.

Aufarbeitung

  1. temperaturethe reaction mixture is refluxed for 20 h
  2. temperatureThe reaction mixture is cooled
  3. customthe solid precipitated
  4. filtrationis filtered
  5. washwashed with water
  6. customdried under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-44595e1950244a75944f176da37f0f04
Quelldatensatz
uspto-grants-2011_12
Patentnummer
US08071597B2

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