Benzoyl Peroxide → HCID 67530800、化合物
反応式
[CH2:1]([O:3][C:4]([C:6]1[O:10][N:9]=[C:8]([CH2:11][CH3:12])[C:7]=1[CH3:13])=[O:5])[CH3:2].C1C(=O)N([Br:21])C(=O)C1.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1>C(Cl)(Cl)(Cl)Cl>[CH2:1]([O:3][C:4]([C:6]1[O:10][N:9]=[C:8]([CH2:11][CH3:12])[C:7]=1[CH2:13][Br:21])=[O:5])[CH3:2]参加物
5
実験手順
3-Ethyl-4-methyl-isoxazole-5-carboxylic acid ethyl ester (3.5 g, 19.1 mmol), NBS (3.4 g, 19.1 mmol), and benzoyl peroxide (0.46 g mg, 1.91 mmol) were added to 110 mL of carbon tetrachloride and the mixture was refluxed for 16 h. The mixture was cooled to room temperature and concentrated in vacuo. The crude product was purified by flash chromatography (0-10% EtOAc/hexanes) to give 1.03 g of the title compound. MS: (+) m/z 262.17, 264.14 (M+1, 79Br/81Br).
後処理
- temperaturethe mixture was refluxed for 16 h
- concentrationconcentrated in vacuo
- customThe crude product was purified by flash chromatography (0-10% EtOAc/hexanes)
出典と根拠
- ORDレコード
- ord-45e336055b7645a18fd671a2f006e7bd
- 出典データセット
- uspto-grants-2012_09
- 特許番号
- US08269008B2
反応ノート
読み込み中…