Triethylamine → 6-Bromo-5-methylpyridine-2-carbonitrile
反応式
[Br:1][C:2]1[C:7]([CH3:8])=[CH:6][CH:5]=[CH:4][N+:3]=1[O-].[CH2:10]([N:12](CC)CC)C.[Si](C#N)(C)(C)C>C(#N)C>[Br:1][C:2]1[N:3]=[C:4]([C:10]#[N:12])[CH:5]=[CH:6][C:7]=1[CH3:8]参加物
5
実験手順
To a solution of 2-bromo-3-methylpyridine 1-oxide (compound 350.1, 5.65 g, 30.1 mmol, 1.00 equiv) in acetonitrile (50 mL) were added triethylamine (6.10 g, 60.3 mmol, 2.00 equiv) and TMSCN (8.90 g, 3.00 equiv). The resulting solution was heated to reflux and stiffed overnight in an oil bath, then cooled to ambient temperature and concentrated under reduced pressure. The residue was purified using silica gel column chromatography with ethyl acetate/petroleum ether (1:5) as eluent to yield 2.00 g (34%) of the title compound as a yellow solid.
後処理
- temperatureThe resulting solution was heated
- temperatureto reflux and stiffed overnight in an oil bath
- concentrationconcentrated under reduced pressure
- customThe residue was purified
出典と根拠
- ORDレコード
- ord-41ecc919343f4ac589479dc8fa7bf9af
- 出典データセット
- uspto-grants-2014_10
- 特許番号
- US08871790B2
反応ノート
読み込み中…