Hydrochloric Acid → 2-Chloro-5-iodo-3-nitropyridine
반응식
[I:1][C:2]1[CH:3]=[C:4]([N+:9]([O-:11])=[O:10])[C:5](N)=[N:6][CH:7]=1.N([O-])=O.[Na+].[NH4+].[OH-].[ClH:18]>Cl[Cu]>[I:1][C:2]1[CH:3]=[C:4]([N+:9]([O-:11])=[O:10])[C:5]([Cl:18])=[N:6][CH:7]=1참가 물질
6
실험 절차
5-iodo-3-nitro-2-aminopyridine (2.511 g, 9.48 mmol) and concentrated HCl (20 mL) were stirred at room temperature for ten minutes. Sodium nitrite (13 g, 188 mmol) was then slowly added followed by CuCl (1.0 g, 10 mmol). Stirring continued overnight. The mixture was poured into 1:1 NH4OH:H2O, extracted with ethyl acetate, dried over sodium sulfate, then concentrated. The crude residue was purified by flash chromatography using 9:1 hexane:ethyl acetate to yield 5-iodo-3-nitro-2-chloropyridine (984 mg, 36%) as a colorless solid.
후처리
- extractionH2O, extracted with ethyl acetate
- dry with materialdried over sodium sulfate
- concentrationconcentrated
- customThe crude residue was purified by flash chromatography
출처 및 근거
- ORD 기록
- ord-9c8d146798a34822a21c69430887e465
- 출처 데이터셋
- uspto-grants-2009_11
- 특허 번호
- US07615567B2
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