Stannous Chloride → (5-Aminopyridin-2-yl)acetonitrile
반응식
[N+:1]([C:4]1[CH:5]=[CH:6][C:7]([CH2:10][C:11]#[N:12])=[N:8][CH:9]=1)([O-])=O.Cl[Sn]Cl>Cl.C(O)C>[NH2:1][C:4]1[CH:5]=[CH:6][C:7]([CH2:10][C:11]#[N:12])=[N:8][CH:9]=1참가 물질
5
실험 절차
To a mixture of (5-nitro-pyridin-2-yl)-acetonitrile (500 mg, 3.06 mmol) in concentrated aqueous HCl (3.1 ml) and ethanol (3.1 ml) at 0° C. SnCl2 (2.3 g, 10.11 mmol) was added. The mixture was allowed to come to room temperature and was stirred for 2 h. The mixture was partitioned between ethyl acetate and saturated aqueous NaHCO3. The aqueous layer was extracted three times with ethyl acetate and the combined organic layers were washed with brine, dried over MgSO4, filtered, and the solvent evaporated under reduced pressure to give the product as a brown oil (300 mg, 74%).
후처리
- customto come to room temperature
- customThe mixture was partitioned between ethyl acetate and saturated aqueous NaHCO3
- extractionThe aqueous layer was extracted three times with ethyl acetate
- washthe combined organic layers were washed with brine
- dry with materialdried over MgSO4
- filtrationfiltered
- customthe solvent evaporated under reduced pressure
출처 및 근거
- ORD 기록
- ord-0057e543d848448d86e6ee868629b03f
- 출처 데이터셋
- uspto-grants-2012_07
- 특허 번호
- US08232426B2
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