反応式
CN([CH:4]=[CH:5][C:6]([CH:8]1[CH2:10][CH2:9]1)=O)C.[N+:11]([CH2:14][C:15]([NH2:17])=[O:16])([O-:13])=[O:12].C([O-])(=O)C.[NH2+]1CCCCC1>O>[CH:8]1([C:6]2[NH:17][C:15](=[O:16])[C:14]([N+:11]([O-:13])=[O:12])=[CH:4][CH:5]=2)[CH2:9][CH2:10]1参加物
5
実験手順
A mixture of crude β-N,N-dimethylaminoethenylcyclopropyl ketone (17-2; 12 g, <86 mmol), nitroacetamide (9 g, 86 mmol) and aqueous piperidinium acetate (10 ml) [prepared from glacial acetic acid (42 ml), water (100 ml) and piperidine (72 ml)] was stirred at room temperature overnight. Following dilution with water (20 ml), the yellow precipitate was isolated via filtration and drying in vacuo to yield the title compound 17-3: 1H NMR (CDCl3) δ 1.15 (m, 2H), 1.36 (m, 2H), 2.10 (m, 1H), 6.02 (br d, J=8.0 Hz, 1H), 8.41 (d, J=8.0 Hz, 1H).
後処理
- customthe yellow precipitate was isolated via filtration
- customdrying in vacuo
出典と根拠
- ORDレコード
- ord-94baea0836ba4ff38a624998dff13d06
- 出典データセット
- uspto-grants-2001_04
- 特許番号
- US06211184B1
関連ノート
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