反応 #11954

ord-556b3489715040888ff745b81e37a366

反応条件

温度
70°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他After the completion of the reaction
  2. 2
    その他the solid was removed
  3. 3
    ろ過filter
  4. 4
    濃縮the filtrate was concentrated
  5. 5
    workup.DISSOLUTIONThe residue was dissolved in chloroform
  6. 6
    洗浄washed with 1 mol/l aqueous solution of sodium hydroxide and saturated brine
  7. 7
    乾燥The solution was dried over anhydrous sodium sulfate
  8. 8
    その他The solvent was removed by distillation
  9. 9
    その他the residue was dried under reduced pressure

実験手順

The compound obtained in Example 17-1 (269.9 mg) was dissolved in carbontetrachloride (8 ml), and N-bromosuccinimide (252.6 mg) and azobisisobutylonitrile (22.1 mg) were added to the solution. The mixture was stirred for 6 hours at 70° C. After the completion of the reaction, the solid was removed using a glass filter and the filtrate was concentrated. The residue was dissolved in chloroform and washed with 1 mol/l aqueous solution of sodium hydroxide and saturated brine. The solution was dried over anhydrous sodium sulfate. The solvent was removed by distillation and the residue was dried under reduced pressure to obtain the title compound (363.3 mg) as pale yellow oil.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07098215B2uspto-grants-2006_08