反应详情

温度

60 °C

Methyl 2-(4-bromophenyl)-2-methylpropanoate (1.29 ml, 5 mmol) was added to 30 ml of 1M aq. NaOH and the mixture was stirred at 60° C. overnight. The solution was acidified with 6M aq. HCl (pH 2) and extracted with EtOAc. The organic extract was washed with brine, dried over MgSO4 and concentrated on vacuum. The crude 2-(4-bromophenyl)-2-methylpropanoic acid was coupled without further purification with 2-methylpropan-1-amine (0.5 ml, 5 mmol) in presence of EDC (1.1 g, 5.5 mmol) and HOBt (675 mg, 5 mmol) in 8 ml of DMF at rt overnight. The mixture was dried down on vacuum and extracted with EtOAc and washed with saturated NaHCO3, 10% citric acid and brine. Organic extracts were dried over MgSO4 and concentrated on vacuum to give 2-(4-bromophenyl)-N-isobutyl-2-methylpropanamide as a white solid (1.4 g, 94%). (M+H, 298).

1. extractionextracted with EtOAc
2. extractionThe organic extract
3. washwas washed with brine
4. dry with materialdried over MgSO4
5. concentrationconcentrated on vacuum
6. customThe mixture was dried down on vacuum
7. extractionextracted with EtOAc
8. washwashed with saturated NaHCO3, 10% citric acid and brine
9. dry with materialOrganic extracts were dried over MgSO4
10. concentrationconcentrated on vacuum