HCID 22024596, Verbindung → HCID 22024494, Verbindung

HRID 1793067Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1793067
[Cl:1][C:2]1[C:3]2[N:4]([C:8]([CH:13]([OH:17])[CH2:14][CH2:15][CH3:16])=[C:9]([CH2:11][CH3:12])[N:10]=2)[CH:5]=[CH:6][N:7]=1>C(OCC)(=O)C.C(Cl)Cl.[O-2].[Mn+4].[O-2]>[Cl:1][C:2]1[C:3]2[N:4]([C:8]([C:13](=[O:17])[CH2:14][CH2:15][CH3:16])=[C:9]([CH2:11][CH3:12])[N:10]=2)[CH:5]=[CH:6][N:7]=1

Komponenten

5

Edukt 1

HCID 22024596HCID 22024596, Verbindung

Produkt 1

HCID 22024494HCID 22024494, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 178418406HCID 178418406, VerbindungKatalysatorHCID 6344DichloromethaneLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

The resulting 1-(8-chloro-2-ethylimidazo[1,2-a]pyrazin-3-yl)-1-butanol was dissolved in ethyl acetate (4 mL) and methylene chloride (1 mL), then activated manganese (IV) oxide (3 g) was added thereto, and the mixture was heated under stirring at 60° C. for 5 hours. After being allowed to cool, the reaction mixture was filtered and washed with ethyl acetate, and then the filtrates were combined and evaporated. The resulting residue was purified by silica gel column chromatography (ethyl acetate:n-hexane=1:3) to give the title compound (226 mg) as white crystals.

Aufarbeitung

  1. temperaturethe mixture was heated
  2. temperatureto cool
  3. filtrationthe reaction mixture was filtered
  4. washwashed with ethyl acetate
  5. customevaporated
  6. customThe resulting residue was purified by silica gel column chromatography (ethyl acetate:n-hexane=1:3)

Quellen und Nachweise

ORD-Eintrag
ord-72159f0f66b74005a17e9d77b719b034
Quelldatensatz
uspto-grants-2006_07
Patentnummer
US07078405B2

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