HCID 18953543, 화합물 → 4-(1H-imidazol-1-yl)pyridin-3-amine
반응식
[N:1]1([C:6]2[CH:11]=[CH:10][N:9]=[CH:8][C:7]=2[N+:12]([O-])=O)[CH:5]=[CH:4][N:3]=[CH:2]1.[H][H]>C(O)C.[C].[Pd]>[NH2:12][C:7]1[CH:8]=[N:9][CH:10]=[CH:11][C:6]=1[N:1]1[CH:5]=[CH:4][N:3]=[CH:2]1참가 물질
5
실험 절차
4-(1-Imidazolyl)-3-nitropyridine (2.10 g, 11.0 mmol) was dissolved in 20 ml of ethanol. After the atmosphere was replaced with nitrogen, 0.25 g of 10% palladium-carbon was added thereto. After the atmosphere was replaced with hydrogen, hydrogen addition was conducted with stirring at room temperature for 3 days. Palladium-carbon was removed by filtration and the filtered cake was washed with ethanol. The filtrate and the washings were combined and then concentrated. The residue was purified by silica gel column chromatography [eluent: dichloromethane: methanol=8:1-6:1 (v/v)] to obtain 1.62 g of a light brown solid (yield: 91.6%).
후처리
- additionwas added
- customPalladium-carbon was removed by filtration
- washthe filtered cake was washed with ethanol
- concentrationconcentrated
- customThe residue was purified by silica gel column chromatography [eluent: dichloromethane: methanol=8:1-6:1 (v/v)]
출처 및 근거
- ORD 기록
- ord-5bff29b70bfc47e88a7c6f72accdcd38
- 출처 데이터셋
- uspto-grants-1993_11
- 특허 번호
- US05262415
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