تفاعل #2069925
ord-c8ffd424e5bb445fb5f64d0847daecbd
معادلة التفاعل
4-Isopropyliodobenzene
N-acetyl-4-isopropylaniline
potassium carbonate
18-crown-6
→
N-Acetyl-N,N-di(4-isopropylphenyl)amine
الكواشف
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1ترشيحthe still-hot reaction mixture is filtered
- 2غسيلthe filter residue is washed thoroughly
- 3أخرىthe solvent is removed on a rotary evaporator
- 4أخرىThe crude product is chromatographed on silica gel using 10% THF in dichloromethane
- 5تركيزThe product fractions are concentrated to dryness
- 6أخرىrecrystallized from hexane
- 7أخرىdried under reduced pressure
الإجراء التجريبي
4-Isopropyliodobenzene (29.2 g, 118 mmol), N-acetyl-4-isopropylaniline (21.0 g, 118 mmol), copper powder (15.0 g, 237 mmol), potassium carbonate (65.4 g, 474 mmol) and 18-crown-6 (2.9 g, 12 mmol) are heated to reflux in 200 ml of 1,2-dichlorobenzene. The reaction is monitored by thin-layer chromatography (eluent: 10% THF in dichloromethane). After 48 h, the still-hot reaction mixture is filtered, the filter residue is washed thoroughly and the solvent is removed on a rotary evaporator. The crude product is chromatographed on silica gel using 10% THF in dichloromethane. The product fractions are concentrated to dryness, recrystallized from hexane and dried under reduced pressure.