N-bromobutanimide → HCID 59828861、化合物
反応式
[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]参加物
5
実験手順
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 (M+).
後処理
- 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)
出典と根拠
- ORDレコード
- ord-01512d9e18ca42dca2e163eee359bf3f
- 出典データセット
- uspto-grants-2011_09
- 特許番号
- US08022062B2
反応ノート
読み込み中…