반응 #7979

ord-194006f950674b50a93e6edc19549752

반응 조건

온도
80°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도After cooling
  2. 2
    기타the mixture was partitioned between EtOAc (20 mL) and water (20 mL)
  3. 3
    세척The organic phase was washed with brine (20 mL)
  4. 4
    건조dried over MgSO4
  5. 5
    여과filtered
  6. 6
    기타evaporated under vacuum

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07087599B2uspto-grants-2006_08