Benzoyl Peroxide → HCID 86686337、化合物
反応式
[Br:1][C:2]1[C:3]([CH3:10])=[N:4][C:5]([CH3:9])=[CH:6][C:7]=1[CH3:8].C1C(=O)N([Br:18])C(=O)C1.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1>C(Cl)(Cl)(Cl)Cl>[Br:1][C:2]1[C:3]([CH2:10][Br:18])=[N:4][C:5]([CH3:9])=[CH:6][C:7]=1[CH3:8]参加物
5
実験手順
A mixture of 3-bromo-2,4,6-trimethylpyridine (15.6 g), NBS (13.9 g) and benzoyl peroxide (567 mg) was heated under reflux in a carbon tetrachloride solvent (300 mL) for two hours. The reaction mixture was cooled to room temperature and then filtered, and the filtration residue was washed with carbon tetrachloride. The resulting filtrate was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (ethyl acetate/n-heptane, 0% to 10%) to give the title compound (3.51 g).
後処理
- temperaturewas heated
- filtrationfiltered
- washthe filtration residue was washed with carbon tetrachloride
- concentrationThe resulting filtrate was concentrated under reduced pressure
- customthe residue was purified by silica gel column chromatography (ethyl acetate/n-heptane, 0% to 10%)
出典と根拠
- ORDレコード
- ord-2f60003e39714ad08b85ed9ead46deec
- 出典データセット
- uspto-grants-2013_10
- 特許番号
- US08563565B2
反応ノート
読み込み中…