Reaktion #473693

ord-b063b26f268341d99b98df2d08e4fb65

Lösungsmittel

Reaktionsbedingungen

Temperatur
50°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe solvent was removed under reduced pressure
  2. 2
    Sonstigethe residue was partitioned between water and ethyl acetate
  3. 3
    ExtraktionThe aqueous layer was extracted twice with ethyl acetate
  4. 4
    WaschenCombined organic extracts were washed with water
  5. 5
    Trocknendried (MgSO4)
  6. 6
    Filtrationfiltered
  7. 7
    EinengenThe filtrate was concentrated under reduced pressure

Vorschrift

A solution of 5-hydroxy-2-adamantanone (2.6 g, 15.66 mmoles) in dichloromethane (DCM) (50 mL) was treated with dimethylaminopyridine (DMAP) (2.1 g, 17 mmoles) and acetic anhydride (2.3 mL, 23 mmoles) and stirred overnight at 50° C. The solvent was removed under reduced pressure and the residue was partitioned between water and ethyl acetate. The aqueous layer was extracted twice with ethyl acetate. Combined organic extracts were washed with water, dried (MgSO4) and filtered. The filtrate was concentrated under reduced pressure to provide the title compound as an off-white solid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08372841B2uspto-grants-2013_02