Phosphorus oxychloride → 6-Chloro-2-methylnicotinonitrile
反応式
[CH3:1][C:2]1[NH:3][C:4](=O)[CH:5]=[CH:6][C:7]=1[C:8]#[N:9].O=P(Cl)(Cl)[Cl:13]>>[Cl:13][C:4]1[CH:5]=[CH:6][C:7]([C:8]#[N:9])=[C:2]([CH3:1])[N:3]=1参加物
3
実験手順
A mixture of 2-Methyl-6-oxo-1,6-dihydro-pyridine-3-carbonitrile (44 g) and POCl3 (250 ml) was refluxed for 3 h. The reaction mixture was dried down in vacuum and ice followed by conc. aqueous ammonia (300 ml) was added. The aqueous layer was extracted with EtOAc. The organic layer was separated, dried and concentrated in vacuum affording the title compound (23.5 g, BP (18 mbar) 119-120° C.).
後処理
- temperaturewas refluxed for 3 h
- customThe reaction mixture was dried down in vacuum and ice
- additionwas added
- extractionThe aqueous layer was extracted with EtOAc
- customThe organic layer was separated
- customdried
- concentrationconcentrated in vacuum
出典と根拠
- ORDレコード
- ord-2b5428a5670845489790d812dc7b0690
- 出典データセット
- uspto-grants-2014_02
- 特許番号
- US08653075B2
反応ノート
読み込み中…