反応 #11954
ord-556b3489715040888ff745b81e37a366
反応方程式
反応条件
温度
70°CELSIUS
詳細条件
See reaction.notes.procedure_details.
後処理
- 1その他After the completion of the reaction
- 2その他the solid was removed
- 3ろ過filter
- 4濃縮the filtrate was concentrated
- 5workup.DISSOLUTIONThe residue was dissolved in chloroform
- 6洗浄washed with 1 mol/l aqueous solution of sodium hydroxide and saturated brine
- 7乾燥The solution was dried over anhydrous sodium sulfate
- 8その他The solvent was removed by distillation
- 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.