반응 #2048852

ord-45469da6908043e29549d371edb62721

반응 조건

온도
50°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The solvent was removed under reduced pressure
  2. 2
    기타the residue was partitioned between water and ethyl acetate
  3. 3
    추출The aqueous layer was extracted twice with ethyl acetate
  4. 4
    세척Combined organic extracts were washed with water
  5. 5
    건조dried (MgSO4)
  6. 6
    여과filtered
  7. 7
    농축The filtrate was concentrated under reduced pressure

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08415354B2uspto-grants-2013_04