反応 #54556

ord-9798e94fd6654119b5add31bf982b1e0

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度under reflux (for 30 min.)
  2. 2
    抽出extracted with chloroform
  3. 3
    その他Desiccation and concentration of the chloroform extracts afforded
  4. 4
    その他a tan solid (1.1 g.), recrystallization of which from acetone

実験手順

A mixture of 1,2,3,4,5,6-hexahydro-6-methyl-8-methoxy-11-oxo-2,6-methano-3-benzazocine (2.18 g.) and hydrobromic acid (48%, 20 ml.) was stirred under reflux (for 30 min.), basified with dilute ammonia and extracted with chloroform. Desiccation and concentration of the chloroform extracts afforded a tan solid (1.1 g.), recrystallization of which from acetone afforded 1,2,3,4,-5,6-hexahydro-6-methyl-8-hydroxy-11-oxo-2,6-methano-3-benzazocine (III: R=CH3, X"=HO, Y+Z=O; 0.4 g.), a white solid.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04149000uspto-grants-1979_04