Nitric Acid → 4-Chloro-3-nitropyridin-2-amine
반응식
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]참가 물질
5
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-d038ee115cd04ba49517293d6c673ecc
- 출처 데이터셋
- uspto-grants-2012_04
- 특허 번호
- US08163767B2
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