Dimethylamine → 5-Bromo-N,N-dimethyl-3-nitropyridin-2-amine
反応式
[Br:1][C:2]1[CH:3]=[C:4]([N+:9]([O-:11])=[O:10])[C:5](Cl)=[N:6][CH:7]=1.[CH3:12][NH:13][CH3:14]>C1COCC1>[Br:1][C:2]1[CH:3]=[C:4]([N+:9]([O-:11])=[O:10])[C:5]([N:13]([CH3:14])[CH3:12])=[N:6][CH:7]=1参加物
4
実験手順
5-Bromo-2-chloro-3-nitropyridine (J. Heterocyclic Chem. 2003, 40, 261) (128 mg, 0.54 mmol) was taken into THF (0.25 mL) followed by addition of 40 W % aqueous dimethylamine (0.25 mL) and the resulting solution was stirred for 1 h at room temperature. The mixture was then partitioned with ethyl ether and 1 M aqueous hydrochloric acid. The organic solution was then washed with additional 1 M aqueous hydrochloric acid (3×) then dried over magnesium sulfate, filtered and concentrated to give 5-bromo-N,N-dimethyl-3-nitropyridin-2-amine. MS (EI) for C7H8N3O2Br: 246, 248 (MH+, Br pattern).
後処理
- customThe mixture was then partitioned with ethyl ether and 1 M aqueous hydrochloric acid
- washThe organic solution was then washed with additional 1 M aqueous hydrochloric acid (3×)
- dry with materialthen dried over magnesium sulfate
- filtrationfiltered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-b79480e94cb64373bd9217576bd72068
- 出典データセット
- uspto-grants-2014_02
- 特許番号
- US08648066B2
反応ノート
読み込み中…