Stannous Chloride → 6-Chloro-N2-methylpyridine-2,3-diamine
반응식
[Cl:1][C:2]1[N:7]=[C:6]([NH:8][CH3:9])[C:5]([N+:10]([O-])=O)=[CH:4][CH:3]=1.[Sn](Cl)Cl.[OH-].[Na+].C(OCC)(=O)C>Cl>[Cl:1][C:2]1[N:7]=[C:6]([NH:8][CH3:9])[C:5]([NH2:10])=[CH:4][CH:3]=1참가 물질
5
실험 절차
6-Chloro-N-methyl-3-nitropyridin-2-amine (1-1, 10.5 g, 56 mmol) and tin(II) chloride dehydrate (50.5 g, 224 mmol) were suspended in concentrated HCl (80 mL) and refluxed overnight. The solution was cooled to room temperature and then added very slowly to a NaOH/ethyl acetate solution at −78° C., until the solution had a slightly basic pH. The suspension was washed with sodium bicarbonate, brine, dried over sodium sulfate, filtered, and concentrated to produce 6-chloro-N2-methylpyridine-2,3-diamine (1-2) as a black solid. HRMS (M+H)+: observed=158.0487, calculated=158.0480.
후처리
- temperaturerefluxed overnight
- washThe suspension was washed with sodium bicarbonate, brine
- dry with materialdried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-64187e08ff7349419fd6ae960a38d822
- 출처 데이터셋
- uspto-grants-2016_04
- 특허 번호
- US09315518B2
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