N-bromobutanimide → 1-Benzyl-2-methyl-5-bromo-1H-imidazole
반응식
[Br:1]N1C(=O)CCC1=O.[CH2:9]([N:16]1[CH:20]=[CH:19][N:18]=[C:17]1[CH3:21])[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1>C(Cl)(Cl)Cl>[CH2:9]([N:16]1[C:20]([Br:1])=[CH:19][N:18]=[C:17]1[CH3:21])[C:10]1[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=1참가 물질
4
실험 절차
Add N-bromosuccinimide (7.85 g, 44 mmol) to a solution of 1-benzyl-2-methyl-1H-imidazole (8.0 g, 46 mmol) in chloroform (200 mL) and stir for 6 hours. Wash reaction with saturated aqueous sodium hydrogen carbonate and saturated aqueous sodium chloride, dry over magnesium sulfate, and filter through 2″ pad of silica gel. Concentrate filtrate reduced pressure. Suspend residue in diethyl ether (600 mL), heat to reflux and filter hot Concentrate ether filtrate under reduced pressure to give 9.3 g (37 mmol) of the desired compound as a tan solid.
후처리
- washWash
- customreaction with saturated aqueous sodium hydrogen carbonate and saturated aqueous sodium chloride
- dry with materialdry over magnesium sulfate
- filtrationfilter through 2″ pad of silica gel
- temperatureSuspend residue in diethyl ether (600 mL), heat
- temperatureto reflux
- filtrationfilter hot
- concentrationConcentrate ether filtrate under reduced pressure
출처 및 근거
- ORD 기록
- ord-f52250e3ee954fa7b57050bbb92284f4
- 출처 데이터셋
- uspto-grants-2011_01
- 특허 번호
- US07863310B2
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