Ethyl Acetate → 5-Bromo-4-methylpyridine-3-carbonitrile
反応式
Br[C:2]1[CH:3]=[N:4][CH:5]=[C:6]([Br:9])[C:7]=1[CH3:8].[C:10]([Cu])#[N:11].CCOC(C)=O>CN(C=O)C>[Br:9][C:6]1[C:7]([CH3:8])=[C:2]([C:10]#[N:11])[CH:3]=[N:4][CH:5]=1参加物
5
実験手順
A mixture of 3,5-dibromo-4-methylpyridine (16 g, 64 mmol) and CuCN (6.2 g, 69 mmol) in 150 mL of DMF was refluxed for 4 hours before cooled down. The reaction mixture was poured to 1 L of EtOAc with stirring and the precipitate was removed by filtration. The filtrate was washed with water, brine, dried over anhydrous Na2SO4 and concentrated. The residue was purified by column chromatography to afford 5-bromo-4-methylpyridine-3-carbonitrile.
後処理
- temperaturewas refluxed for 4 hours
- temperaturebefore cooled down
- customthe precipitate was removed by filtration
- washThe filtrate was washed with water, brine
- dry with materialdried over anhydrous Na2SO4
- concentrationconcentrated
- customThe residue was purified by column chromatography
出典と根拠
- ORDレコード
- ord-5de5469c8b0e4c90afecc837e125c4d2
- 出典データセット
- uspto-grants-2015_12
- 特許番号
- US09206199B2
反応ノート
読み込み中…