Phosphorus oxychloride → 3-Chloro-6-(4-methoxyphenyl)pyridazine
反応式
P(Cl)(Cl)([Cl:3])=O.[CH3:6][O:7][C:8]1[CH:13]=[CH:12][C:11]([C:14]2[N:19]=[N:18][C:17](O)=[CH:16][CH:15]=2)=[CH:10][CH:9]=1>O>[Cl:3][C:17]1[N:18]=[N:19][C:14]([C:11]2[CH:12]=[CH:13][C:8]([O:7][CH3:6])=[CH:9][CH:10]=2)=[CH:15][CH:16]=1参加物
4
実験手順
With cooling with ice, 50 ml of phosphorus oxychloride was added to 10.00 g (49.5 mmol) of the obtained 6-(4-methoxyphenyl)-pyridazin-3-ol, and the reaction liquid was stirred under reflux for 6 hours. Water was added to the reaction liquid, extracted with chloroform, and the organic layer was washed with saturated saline water. This was dried with anhydrous sodium sulfate, and concentrated under reduced pressure to obtain 4.41 g (yield: 40%) of 3-chloro-6-(4-methoxyphenyl)-pyridazine as a white solid.
後処理
- customthe reaction liquid
- temperatureunder reflux for 6 hours
- extractionextracted with chloroform
- washthe organic layer was washed with saturated saline water
- dry with materialThis was dried with anhydrous sodium sulfate
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-936e47842d8540a98e4314fa99ceaf21
- 出典データセット
- uspto-grants-2010_01
- 特許番号
- US07645756B2
反応ノート
読み込み中…