Reaktion #7979

ord-194006f950674b50a93e6edc19549752

Lösungsmittel

Reaktionsbedingungen

Temperatur
80°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturAfter cooling
  2. 2
    Sonstigethe mixture was partitioned between EtOAc (20 mL) and water (20 mL)
  3. 3
    WaschenThe organic phase was washed with brine (20 mL)
  4. 4
    Trocknendried over MgSO4
  5. 5
    Filtrationfiltered
  6. 6
    Sonstigeevaporated under vacuum

Vorschrift

The product from step 1 in ethanol (1.0 mL), water (0.2 mL) and aqueous 2N HCl (0.2 mL) was stirred and heated in an oil bath at 80° C. for 40 minutes. After cooling, the mixture was partitioned between EtOAc (20 mL) and water (20 mL). The organic phase was washed with brine (20 mL), dried over MgSO4, filtered, and evaporated under vacuum to provide 4-acetyl-9a-butyl-8-chloro-7-methoxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one (54 mg) as an oil.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07087599B2uspto-grants-2006_08