反応 #7979

ord-194006f950674b50a93e6edc19549752

反応条件

温度
80°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度After cooling
  2. 2
    その他the mixture was partitioned between EtOAc (20 mL) and water (20 mL)
  3. 3
    洗浄The organic phase was washed with brine (20 mL)
  4. 4
    乾燥dried over MgSO4
  5. 5
    ろ過filtered
  6. 6
    その他evaporated under vacuum

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07087599B2uspto-grants-2006_08