반응 #69961

ord-0037591a615e4fe095b275a6c05ed8ab

반응 조건

온도
60°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도to cool down to room temperature
  2. 2
    workup.WAITleft
  3. 3
    농축The reaction mixture is concentrated under reduced pressure
  4. 4
    workup.DISSOLUTIONdissolved in ethyl acetate (200 ml)
  5. 5
    세척washed with aqueous 2N sodium carbonate (100 ml)
  6. 6
    건조The organic layer is then dried over magnesium sulphate
  7. 7
    농축concentrated under reduced pressure

실험 절차

To a suspension of 10-oxa-tricyclo[5.2.1.0*2,6*]decane-3,5-dione (9.97 g, 60 mmol) in methanol (200 ml) is added sodium tetrachloroaurate (597 mg, 1.5 mmol) and the reaction mixture is heated to 60° C. for 7 hours. The reaction mixture is allowed to cool down to room temperature and left to stand overnight. The reaction mixture is concentrated under reduced pressure, dissolved in ethyl acetate (200 ml) and washed with aqueous 2N sodium carbonate (100 ml), followed by saturated brine (100 ml). The organic layer is then dried over magnesium sulphate and concentrated under reduced pressure to give 5-methoxy-10-oxa-tricyclo[5.2.1.0*2,6*]dec-4-en-3-one (8.62 g)

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08530667B2uspto-grants-2013_09