N-bromobutanimide → HCID 59828861, 화합물
반응식
[CH3:1][CH:2]([CH3:13])[CH2:3][C:4]([C:6]1[CH:11]=[CH:10][C:9]([CH3:12])=[CH:8][CH:7]=1)=[O:5].C1C(=O)N([Br:21])C(=O)C1>C(Cl)(Cl)(Cl)Cl.CC(N=NC(C#N)(C)C)(C#N)C>[CH3:1][CH:2]([CH3:13])[CH2:3][C:4]([C:6]1[CH:7]=[CH:8][C:9]([CH2:12][Br:21])=[CH:10][CH:11]=1)=[O:5]참가 물질
5
실험 절차
Heat a mixture of 3,4′-dimethylbutyrophenone (3 g, 17.02 mmol), NBS (3.787 g, 16.18 mmol), and AIBN (70 mg, 0.425 mmol) in carbon tetrachloride (80 mL) for 14 h at reflux. Cool to ambient temperature and filter the mixture. Concentrate the filtrate in vacuo. Purify the crude mixture by chromatography on silica gel eluting sequentially with hexane and hexane/EtOAc (9:1) to provide the title compound as oil (2.802 g, 65%). GC-MS m/z: 255 (Ma).
후처리
- temperatureHeat
- temperatureat reflux
- filtrationfilter the mixture
- concentrationConcentrate the filtrate in vacuo
- customPurify the crude mixture by chromatography on silica gel eluting sequentially with hexane and hexane/EtOAc (9:1)
출처 및 근거
- ORD 기록
- ord-2eff0da1019f47c88965b7875961ecb2
- 출처 데이터셋
- uspto-grants-2013_11
- 특허 번호
- US08580780B2
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