3-Acetylpyridine → 1-(3-Pyridinyl)ethanone oxime
反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([C:7](=O)[CH3:8])[CH:2]=1.Cl.[NH2:11][OH:12].C(=O)(O)[O-].[Na+]>CO.O>[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([C:7](=[N:11][OH:12])[CH3:8])[CH:2]=1参加物
6
実験手順
A mixture of 50 g (0.41 mol) of 1-(3-pyridinyl)ethanone and 29 g (0.42 mol) of hydroxylamine hydrochloride in 250 ml of methanol was heated under reflux for five hours. Upon cooling to room temperature, a white solid separated from the reaction mixture. This material was collected by filtration and the filtrate was concentrated to yield additional white solid. The combined solids were dissolved in water and the solution was made weakly basic by the addition of sodium bicarbonate solution while cooling. The white precipitate which formed was separated by filtration to yield 55.4 g of 1-(3-pyridinyl)ethanone oxime, mp 115°-117° C.
後処理
- temperaturewas heated
- temperatureunder reflux for five hours
- customa white solid separated from the reaction mixture
- filtrationThis material was collected by filtration
- concentrationthe filtrate was concentrated
- customto yield additional white solid
- temperaturewhile cooling
- customThe white precipitate which formed
- customwas separated by filtration
出典と根拠
- ORDレコード
- ord-75b0ea45e2d44afd9c028f284a7311b7
- 出典データセット
- uspto-grants-1987_12
- 特許番号
- US04710508
反応ノート
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