Bromine → 2-bromo-1-(6-bromopyridin-3-yl)ethanone
反応式
[Br:1][C:2]1[N:7]=[CH:6][C:5]([C:8](=[O:10])[CH3:9])=[CH:4][CH:3]=1.[Br:11]Br>C(Cl)(Cl)Cl.C([O-])(O)=O.[Na+].[Cl-].[Al+3].[Cl-].[Cl-]>[Br:11][CH2:9][C:8]([C:5]1[CH:6]=[N:7][C:2]([Br:1])=[CH:3][CH:4]=1)=[O:10]参加物
6
実験手順
To a solution of 1-(6-bromo-pyridin-3-yl)-ethanone (20.3 g, 101 mmol) and aluminum chloride (200 mg, 1.5 mmol) in chloroform (288 mL) was added bromine (5.23 mL, 101 mmol). The mixture was stirred at rt for 16 h. Upon completion of the reaction as judged by LC/MS analysis, the solution was diluted with sat aq NaHCO3 and extracted with DCM. The organic layer was removed, dried over MgSO4, filtered and concentrated giving rise to 31 g 2-bromo-1-(6-bromopyridin-3-yl)ethanone, which was taken on immediately. LC/MS: m/e 277.9 (M+H).
後処理
- customUpon completion of the reaction
- extractionextracted with DCM
- customThe organic layer was removed
- dry with materialdried over MgSO4
- filtrationfiltered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-1d877aec02d04f359906a8f4a9add368
- 出典データセット
- uspto-grants-2014_03
- 特許番号
- US08673941B2
反応ノート
読み込み中…