3-Acetylpyridine → 1-(3-Pyridinyl)-1-ethanone hydrazone
反応式
[C:1]([C:4]1[CH:5]=[N:6][CH:7]=[CH:8][CH:9]=1)(=O)[CH3:2].O.O.[NH2:12][NH2:13]>O>[N:6]1[CH:7]=[CH:8][CH:9]=[C:4]([C:1](=[N:12][NH2:13])[CH3:2])[CH:5]=1参加物
4
実験手順
To 3-acetylpyridine (6.1 g, 52 mmol) in industrial methylated spirits (50 ml) was added dropwise hydrazine hydrate monohydrate (3.11 ml, 0.1 mol). The reaction mixture was refluxed for 4 h, before cooling to room temperature and stirring for 16 h. Water (25 ml) was added and the volatile organics were removed in vacuo. The predominantly aqueous residual liquor was extracted with ethyl acetate, and the combined organic extracts were dried (Na2SO4) and concentrated to give a yellow oil (5.4 g, 80%) which was taken forward without further purification.
後処理
- temperatureThe reaction mixture was refluxed for 4 h
- customthe volatile organics were removed in vacuo
- extractionThe predominantly aqueous residual liquor was extracted with ethyl acetate
- dry with materialthe combined organic extracts were dried (Na2SO4)
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-038c360d8d524b7cae77a7c6c57cefe8
- 出典データセット
- uspto-grants-2001_11
- 特許番号
- US06313312B1
反応ノート
読み込み中…