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+].[OH-].[NH4+].O.[ClH:19]>[Cu]Cl>[Cl:19][C:5]1[C:4]([N+:9]([O-:11])=[O:10])=[CH:3][C:2]([I:1])=[CH:7][N:6]=1参加物
7
実験手順
To a solution of 5-iodo-3-nitropyridin-2-amine (1.3 g, 4.9 mmol) in concentrated HCl at 0° C. was added sodium nitrite (6.73 g, 97.13 mmol, 20 eq.) stepwise followed by the addition of copper(I) chloride (0.5 g, 4.9 mmol, 1 eq.) and the mixture was stirred at RT for 12 h. The mixture was then poured in to a mixture of ammonium hydroxide and water (1:1) and extracted with ethylacetate (3×150 ml). The combined organic layer was washed with water, aqueous sodium thiosulfate, brine and dried over sodium sulphate. The solvent was distilled off to afford the product in 43% yield (0.6 g).
後処理
- extractionextracted with ethylacetate (3×150 ml)
- washThe combined organic layer was washed with water, aqueous sodium thiosulfate, brine
- dry with materialdried over sodium sulphate
- distillationThe solvent was distilled off
- customto afford the product in 43% yield (0.6 g)
出典と根拠
- ORDレコード
- ord-fd868a0cfcec4c8d8f246e32aeb9792f
- 出典データセット
- uspto-grants-2016_09
- 特許番号
- US09447091B2
反応ノート
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