Hydrogen Peroxide → 5-Methoxy-2-methyl-1-oxo-1lambda~5~-pyridine

HRID 845533Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 845533
[OH:1]O.[CH3:3][O:4][C:5]1[CH:6]=[CH:7][C:8]([CH3:11])=[N:9][CH:10]=1>C(O)(=O)C>[CH3:3][O:4][C:5]1[CH:6]=[CH:7][C:8]([CH3:11])=[N+:9]([O-:1])[CH:10]=1

Komponenten

4

Edukt 2

HCID 784Hydrogen PeroxideHCID 133587775-Methoxy-2-methylpyridine

Produkt 1

HCID 122140195-Methoxy-2-methyl-1-oxo-1lambda~5~-pyridineAusbeute 77 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

120 g of 30% strength hydrogen peroxide solution are added dropwise to a solution of 60.9 g of 5-methoxy-2-methylpyridine in 300 ml of glacial acetic acid at 60° C. in the course of 1 hour and the mixture is subsequently stirred for 3 hours. After destruction of excess per-compounds by addition of active manganese dioxide, the mixture is filtered, the filtrate is concentrated, the residue is clarified hot in 500 ml of ethyl acetate, the mixture is concentrated again and the residue is distilled under 0.3 mbar. 54 g (77% of theory) of 5-methoxy-2-methylpyridine 1-oxide are obtained as a rapidly solidifying oil (b.p. 130° C.); m.p. 80°-84° C.

Aufarbeitung

  1. customAfter destruction of excess per-compounds
  2. additionby addition of active manganese dioxide
  3. filtrationthe mixture is filtered
  4. concentrationthe filtrate is concentrated
  5. concentrationthe mixture is concentrated again
  6. distillationthe residue is distilled under 0.3 mbar

Quellen und Nachweise

ORD-Eintrag
ord-cb46f12517d842b19906d830bd4b49e3
Quelldatensatz
uspto-grants-1988_07
Patentnummer
US04758579

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