Phosphorus pentachloride → 6-chloro-5-nitronicotinonitrile
반응식
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]=1참가 물질
4
반응 조건
- 온도
- 130 °C
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-c1566577dfda4a5490cc50ad67a4dd21
- 출처 데이터셋
- uspto-grants-2003_06
- 특허 번호
- US06582351B1
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