Nitric Acid → 4-Chloro-3-nitropyridin-2-amine
反応式
Cl.[Cl:2][C:3]1[CH:8]=[CH:7][N:6]=[C:5]([NH2:9])[CH:4]=1.S(=O)(=O)(O)O.[N+:15]([O-])([OH:17])=[O:16]>O>[Cl:2][C:3]1[CH:8]=[CH:7][N:6]=[C:5]([NH2:9])[C:4]=1[N+:15]([O-:17])=[O:16]参加物
5
実験手順
4-Chloro-2-pyridinamine hydrochloride (300 mg) was added portionwise to concentrated sulfuric acid (1.96 mL) at 4° C. To the mixture was added fuming nitric acid (0.1 mL) dropwise at 4° C. The mixture was stirred at ambient temperature for 3 hours. To the solution was added water and the mixture was extracted with EtOAc. The extract was washed with water, dried over MgSO4 and concentrated under reduced pressure. The residue was purified by column chromatography on silica gel with EtOAc and n-hexane to give 4-chloro-3-nitro-2-pyridinamine (125 mg) as a yellow powder.
後処理
- extractionthe mixture was extracted with EtOAc
- washThe extract was washed with water
- dry with materialdried over MgSO4
- concentrationconcentrated under reduced pressure
- customThe residue was purified by column chromatography on silica gel with EtOAc and n-hexane
出典と根拠
- ORDレコード
- ord-d038ee115cd04ba49517293d6c673ecc
- 出典データセット
- uspto-grants-2012_04
- 特許番号
- US08163767B2
反応ノート
読み込み中…