Benzoyl Peroxide → 3-Bromo-2-(bromomethyl)-6-methoxy-4-methylpyridine
反応式
[Br:1][C:2]1[C:3]([CH3:11])=[N:4][C:5]([O:9][CH3:10])=[CH:6][C:7]=1[CH3:8].C1C(=O)N([Br:19])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]([CH2:11][Br:19])=[N:4][C:5]([O:9][CH3:10])=[CH:6][C:7]=1[CH3:8]参加物
5
実験手順
A mixture of 3-bromo-6-methoxy-2,4-dimethylpyridine obtained in Preparation Example 22 (200 mg), NBS (165 mg) and benzoyl peroxide (6.73 mg) was heated under reflux in a carbon tetrachloride solvent (4 mL) for two hours. The reaction mixture was cooled to room temperature and then filtered. The resulting filtrate was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (ethyl acetate/n-heptane, 0% to 5%) to give the title compound (126 mg).
後処理
- temperaturewas heated
- filtrationfiltered
- concentrationThe resulting filtrate was concentrated under reduced pressure
- customthe residue was purified by silica gel column chromatography (ethyl acetate/n-heptane, 0% to 5%)
出典と根拠
- ORDレコード
- ord-590b71fa388c4a8fa285bcde42713374
- 出典データセット
- uspto-grants-2013_10
- 特許番号
- US08563565B2
反応ノート
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