Triethylamine → HCID 178477995、化合物
反応式
[Cl:1][C:2]1[S:6][C:5]([C:7](=O)[C:8]([C:13]2[CH:18]=[CH:17][N:16]=[CH:15][CH:14]=2)=[CH:9][N:10](C)C)=[CH:4][CH:3]=1.O.NN.C([N:25](CC)CC)C>C(O)C>[Cl:1][C:2]1[S:6][C:5]([C:7]2[C:8]([C:13]3[CH:18]=[CH:17][N:16]=[CH:15][CH:14]=3)=[CH:9][NH:10][N:25]=2)=[CH:4][CH:3]=1参加物
5
実験手順
A mixture of 1-(5-chloro-2-thienyl)-3-(dimethylamino)-2-(pyridin-4-yl)prop-2-en-1-one (5.1 mmol), hydrazine hydrate (7.6 mmol) and triethylamine (7.6 mmol) in 25 mL ethanol was refluxed for 3 h. The solvent was evaporated under reduced pressure and the residue was purified by chromatography on silica gel (dichloromethane:methanol 50:1 to 20:1) to afford 1.16 g 4-[3-(5-chloro-2-thienyl)-1H-pyrazol-4-yl]pyridine (83% yield).
後処理
- temperaturewas refluxed for 3 h
- customThe solvent was evaporated under reduced pressure
- customthe residue was purified by chromatography on silica gel (dichloromethane:methanol 50:1 to 20:1)
出典と根拠
- ORDレコード
- ord-35a18591063d4b50b3151267f29689aa
- 出典データセット
- uspto-grants-2014_04
- 特許番号
- US08685974B2
反応ノート
読み込み中…