Reaktion #42866

ord-864196ae632e4aceaa2104297d6f9e87

Reaktionsgleichung

COc1cc2c(cc1O)-c1c(C)c3ccc4c(c3c[n+]1CC2)OCO4.COc1cc2c(cc1OC)-c1c(C)c3ccc4c(c3c[n+]1CC2)OCO4.[Cl-]
dehydrocavidine dehydroapocavidine
→
COc1cc2c(cc1OC)-c1c(C)c3ccc4c(c3c[n+]1CC2)OCO4.[Cl-]
dehydrocavidine
COc1cc2c(cc1O)-c1c(C)c3ccc4c(c3c[n+]1CC2)OCO4
dehydroapocavidine

Edukte

COc1cc2c(cc1O)-c1c(C)c3ccc4c(c3c[n+]1CC2)OCO4.COc1cc2c(cc1OC)-c1c(C)c3ccc4c(c3c[n+]1CC2)OCO4.[Cl-]
dehydrocavidine dehydroapocavidine
—
sephadex

Reagenzien

Keine

Lösungsmittel

CO
methanol

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Waschena gradient elution
  2. 2
    workup.ADDITIONThe eluate containing dehydrocavidine
  3. 3
    Einengenis then concentrated by decompression to a constant weight
  4. 4
    Sonstigeresulting

Vorschrift

200 mg of the dehydrocavidine-dehydroapocavidine composition obtained from the above step is dissolved with 10 ml of methanol, and are then loaded to the top of the sephadex gel column, and a gradient elution is employed with 30%˜70% methanol, accompanied by TLC tracking. The eluate containing dehydrocavidine is combined and is then concentrated by decompression to a constant weight, resulting in obtaining 22 mg of a dehydrocavidine compound and 14 mg of a dehydroapocavidine compound respectively.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07732458B2uspto-grants-2010_06