反応 #49274
ord-7387e8246d2a488ebc482fbdeadd6168
溶媒
反応条件
詳細条件
See reaction.notes.procedure_details.
後処理
- 1抽出extracted with ethyl acetate
- 2洗浄The organic layer was washed with 0.5 mol/L hydrochloric acid and saturated brine
- 3乾燥dried over anhydrous sodium sulfate
- 4その他The solvent was evaporated under reduced pressure
- 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%).