Hydrochloric Acid → 2-Chloro-5-iodo-3-nitropyridine
反応式
[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]=1参加物
6
実験手順
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.
後処理
- extractionH2O, extracted with ethyl acetate
- dry with materialdried over sodium sulfate
- concentrationconcentrated
- customThe crude residue was purified by flash chromatography
出典と根拠
- ORDレコード
- ord-9c8d146798a34822a21c69430887e465
- 出典データセット
- uspto-grants-2009_11
- 特許番号
- US07615567B2
反応ノート
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