Hydrazine hydrate (1:1) → 6-(4-Fluorophenyl)-4,5-dihydro-3(2H)-pyridazinone
反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=O)[CH2:9][CH2:10][C:11]([OH:13])=O)=[CH:4][CH:3]=1.O.[NH2:16][NH2:17]>C(O)C>[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH2:9][CH2:10][C:11](=[O:13])[NH:16][N:17]=2)=[CH:4][CH:3]=1参加物
4
反応条件
- 温度
- 80 °C
実験手順
In a round-bottomed flask, 4-(4-fluoro-phenyl)-4-oxo-butyric acid (4.90 g, 25.0 mmol) and hydrazine hydrate (1.70 ml, 35.0 mmol) were dissolved in ethanol (50 ml), and the reaction mixture was heated to about 80° C. for about ninety minutes. The mixture was allowed to cool to room temperature and then concentrated in vacuo. The resulting solids were suspended and stirred in ethanol (10 ml) for ten minutes and the mixture was then filtered to give pure product (4.14 g, 21.5 mmol, 86% yield). LRMS ([M+H]+)=193.2; m.p. 191-193° C.
後処理
- temperatureto cool to room temperature
- concentrationconcentrated in vacuo
- filtrationthe mixture was then filtered
出典と根拠
- ORDレコード
- ord-a9cbcc58b91b4de7bff44c4f7c077059
- 出典データセット
- uspto-grants-2003_05
- 特許番号
- US06566377B2
反応ノート
読み込み中…