Phosphorus pentachloride → 6-chloro-5-nitronicotinonitrile
反応式
O[C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[CH:9][C:5]([C:6]([NH2:8])=O)=[CH:4][N:3]=1.P(Cl)(Cl)(Cl)(Cl)[Cl:15]>P(Cl)(Cl)(Cl)=O>[Cl:15][C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[CH:9][C:5]([C:6]#[N:8])=[CH:4][N:3]=1参加物
4
反応条件
- 温度
- 130 °C
実験手順
A mixture of 6-hydroxy-5-nitronicotinamide (343 g), phosphorus oxychloride (40 ml) and phosphorus pentachloride (1287 g) was heated at 130° C. for 3.5 hours. After cooling to ambient temperature, the mixture was concentrated in vacuo. The residue was partitioned between ethyl acetate and an aqueous saturated sodium bicarbonate solution. The organic layer was dried over magnesium sulfate and evaporated to afford 6-chloro-5-nitronicotinonitrile (374 g) as an oil.
後処理
- temperatureAfter cooling to ambient temperature
- concentrationthe mixture was concentrated in vacuo
- customThe residue was partitioned between ethyl acetate
- dry with materialThe organic layer was dried over magnesium sulfate
- customevaporated
出典と根拠
- ORDレコード
- ord-c1566577dfda4a5490cc50ad67a4dd21
- 出典データセット
- uspto-grants-2003_06
- 特許番号
- US06582351B1
反応ノート
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