反応 #49274

ord-7387e8246d2a488ebc482fbdeadd6168

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    抽出extracted with ethyl acetate
  2. 2
    洗浄The organic layer was washed with 0.5 mol/L hydrochloric acid and saturated brine
  3. 3
    乾燥dried over anhydrous sodium sulfate
  4. 4
    その他The solvent was evaporated under reduced pressure
  5. 5
    その他the residue was purified by slurry

実験手順

Iodine (6.29 g, 24.8 mmol) was dissolved in ethanol (225 mL), and the solution was added with silver sulfate (3.87 g, 12.4 mmol) and 3-amino-6-bromophthalimide (3.00 g, 12.4 mmol), followed by stirring at room temperature for 23 hours. The reaction mixture was added with 10% aqueous sodium thiosulfate solution and extracted with ethyl acetate. The organic layer was washed with 0.5 mol/L hydrochloric acid and saturated brine and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, the residue was purified by slurry using hexane and methanol to obtain 3-amino-4-iodo-6-bromophthalimide (4.3 g. yield 96%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07745641B2uspto-grants-2010_06