Phosphorus oxychloride → 2-Chloro-3-iodo-5-nitropyridine
반응식
[I:1][C:2]1[C:3](O)=[N:4][CH:5]=[C:6]([N+:8]([O-:10])=[O:9])[CH:7]=1.O=P(Cl)(Cl)[Cl:14].P(Cl)(Cl)(Cl)(Cl)Cl>O>[Cl:14][C:3]1[C:2]([I:1])=[CH:7][C:6]([N+:8]([O-:10])=[O:9])=[CH:5][N:4]=1참가 물질
5
반응 조건
- 온도
- 140 °C
실험 절차
A mixture of 3-iodo-5-nitropyridin-2-ol (37.6 mmol, 10 g), POCl3 (86.47 mmol, 7.94 ml) and PCl5 (48.87 mmol, 10.2 g) was heated at 140° C. for 1 h, under argon atmosphere. The crude mixture was poured into a mixture of ice and water and extracted with DCM. The solid residue was purified by chromatography over SiO2 eluting with hexane/dichloromethane mixtures affording 2-chloro-3-iodo-5-nitropyridine (7.32 g, yield 69%) of the expected product.
후처리
- extractionextracted with DCM
- customThe solid residue was purified by chromatography over SiO2 eluting with hexane/dichloromethane
출처 및 근거
- ORD 기록
- ord-36430576da66434ab6f7608884f5d2a3
- 출처 데이터셋
- uspto-grants-2013_09
- 특허 번호
- US08536165B2
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