HCID 18953543、化合物 → 4-(1H-imidazol-1-yl)pyridin-3-amine
反応式
[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]1参加物
5
実験手順
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%).
後処理
- 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)]
出典と根拠
- ORDレコード
- ord-5bff29b70bfc47e88a7c6f72accdcd38
- 出典データセット
- uspto-grants-1993_11
- 特許番号
- US05262415
反応ノート
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