反応式
N/[C:2](=[CH:5]\[CH3:6])/[C:3]#[N:4].[NH:7]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][N:10]=1)[NH2:8].C(O)(=O)C>C(O)C>[CH3:6][C:5]1[CH:2]=[C:3]([NH2:4])[N:7]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][N:10]=2)[N:8]=1参加物
実験手順
To an ice-cold solution of aminocrotononitrile (82 g, 1.0 mol) and 2-hydrazinopyridine (120 g, 1.1 mol) in ethanol (300 mL) was added acetic acid (132 g, 2.2 mol), and the mixture was heated under reflux for 3.5 hours. After the mixture was allowed to cool to room temperature, the reaction solvent was evaporated under reduced pressure and water was added to the residue. After the solution was made basic by the addition of an aqueous sodium hydroxide solution, organic matter was extracted with ethyl acetate. The extract was washed with saturated brine and water and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. Purification of the residue by silica gel column chromatography (ethyl acetate) gave the title compound (156.3 g, 90% yield).
後処理
- temperaturethe mixture was heated
- temperatureunder reflux for 3.5 hours
- customthe reaction solvent was evaporated under reduced pressure and water
- additionwas added to the residue
- additionAfter the solution was made basic by the addition of an aqueous sodium hydroxide solution, organic matter
- extractionwas extracted with ethyl acetate
- washThe extract was washed with saturated brine and water
- dry with materialdried over anhydrous magnesium sulfate
- customthe solvent was evaporated under reduced pressure
- customPurification of the residue by silica gel column chromatography (ethyl acetate)
出典と根拠
- ORDレコード
- ord-608a2beee47140a2a93a373efc43f977
- 出典データセット
- uspto-grants-2005_09
- 特許番号
- US06949648B2
関連ノート
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