Phosphorus oxychloride → 3-Acetyl-4-chloro-8-methoxyquinoline
反応式
[C:1]([C:4]1[C:13](=O)[C:12]2[C:7](=[C:8]([O:15][CH3:16])[CH:9]=[CH:10][CH:11]=2)[NH:6][CH:5]=1)(=[O:3])[CH3:2].P(Cl)(Cl)([Cl:19])=O>>[C:1]([C:4]1[CH:5]=[N:6][C:7]2[C:12]([C:13]=1[Cl:19])=[CH:11][CH:10]=[CH:9][C:8]=2[O:15][CH3:16])(=[O:3])[CH3:2]参加物
3
実験手順
3-Acetyl-8-methoxy-4(1H)-quinolone (4.23 g, 19 mmol) and phosphorus oxychloride (150 ml) were heated under reflux for 45 minutes, evaporated to small volume in vacuo, poured onto ice, and the mixture adjusted to pH 4 with sodium bicarbonate. Extraction with chloroform, drying and evaporation of the organic solution gave crude 3-acetyl-4-chloro-8-methoxyquinoline as a dark coloured oil (7.9 g), which was used without purification.
後処理
- temperatureunder reflux for 45 minutes
- customevaporated to small volume in vacuo
- additionpoured onto ice
- extractionExtraction with chloroform
- customdrying
- customevaporation of the organic solution
出典と根拠
- ORDレコード
- ord-40ac11edc0ee40bf8259deefd3ab5374
- 出典データセット
- uspto-grants-1989_02
- 特許番号
- US04806550
反応ノート
読み込み中…