Phosphorus oxychloride → 5-Acetyl-3-pyridinecarbonitrile
反応式
P(Cl)(Cl)(Cl)=O.[C:6]([C:9]1[CH:10]=[N:11][CH:12]=[C:13]([C:15](=O)[NH2:16])[CH:14]=1)(=[O:8])[CH3:7]>CN(C)C=O>[C:6]([C:9]1[CH:10]=[N:11][CH:12]=[C:13]([C:15]#[N:16])[CH:14]=1)(=[O:8])[CH3:7]参加物
4
実験手順
Phosphorus oxychloride (2.75 g) was added to a solution of 3-acetyl-5-carbamoylpyridine (2.8 g) in N,N-dimethylformamide (30 ml) with cooling on an ice-water bath. The mixture was stirred with cooling for 1.5 hours. The solvent was removed under reduced pressure. The residue was dissolved in water (150 ml) and the mixture was extracted with ethyl acetate (100 ml). The extract was dried with magnesium sulfate and then evaporated. The residue was chromatographed on a silica gel column eluting with chloroform to afford 3-acetyl-5-cyanopyridine (1.21 g).
後処理
- temperaturewith cooling on an ice-water bath
- temperaturewith cooling for 1.5 hours
- customThe solvent was removed under reduced pressure
- dissolutionThe residue was dissolved in water (150 ml)
- extractionthe mixture was extracted with ethyl acetate (100 ml)
- dry with materialThe extract was dried with magnesium sulfate
- customevaporated
- customThe residue was chromatographed on a silica gel column
- washeluting with chloroform
出典と根拠
- ORDレコード
- ord-c7a44f96e5cc4d408dd1ebcf43f7f1f2
- 出典データセット
- uspto-grants-1994_11
- 特許番号
- US05364871
反応ノート
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