反応 #1605812
ord-c1a270181535486187596470ab6be54a
反応条件
詳細条件
See reaction.notes.procedure_details.
後処理
- 1濃縮The solution was concentrated under reduced pressure, to the residue
- 2workup.ADDITIONwas added water (20 mL) and subsequently ethanol (30 mL)
- 3workup.STIRRINGthe mixture was stirred under ice bath for 1 hour
- 4ろ過The precipitate was collected by filtration
- 5洗浄washed with ethanol/water (=1:1)
- 6その他dried under reduced pressure
実験手順
2-Phenyl-N-acetylaniline (6.21 g, 29.40 mmol) was dissolved in acetic acid (70 mL). Thereto was dropwise added under ice bath a separately prepared solution of hydrogen bromide (6.14 g, 38.42 mmol) dissolved in carbon tetrachloride (19.21 mL) and the mixture was stirred at room temperature overnight. The solution was concentrated under reduced pressure, to the residue was added water (20 mL) and subsequently ethanol (30 mL), and the mixture was stirred under ice bath for 1 hour. The precipitate was collected by filtration, washed with ethanol/water (=1:1), dried under reduced pressure to obtain 2-phenyl-4-bromo-N-acetylaniline (7.79 g).