Phosphorus oxychloride → 4,6-Dichloro-3-nitroquinoline
反応式
[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]=[CH:7][C:6]([N+:12]([O-:14])=[O:13])=[C:5]2O.O=P(Cl)(Cl)[Cl:18]>>[Cl:18][C:5]1[C:4]2[C:9](=[CH:10][CH:11]=[C:2]([Cl:1])[CH:3]=2)[N:8]=[CH:7][C:6]=1[N+:12]([O-:14])=[O:13]参加物
3
実験手順
6-Chloro-3-nitroquinolin-4-ol (Compound of step 2, 5 g, 22.42 mmol) in POCl3 (150 mL, 493 mmol) was stirred for 45 min at 120° C. The mixture was cooled to RT and poured slowly into ice-water. The precipitate was filtered, washed with ice-cold water, and dissolved in CH2Cl2. The organic phase was washed with cold brine and dried over Na2SO4. The organic solvent was evaporated to dryness to obtain the title compound.
後処理
- filtrationThe precipitate was filtered
- washwashed with ice-cold water
- dissolutiondissolved in CH2Cl2
- washThe organic phase was washed with cold brine
- dry with materialdried over Na2SO4
- customThe organic solvent was evaporated to dryness
出典と根拠
- ORDレコード
- ord-8e3351cd1f964ade91403170bb04b6e9
- 出典データセット
- uspto-grants-2014_01
- 特許番号
- US08637670B2
反応ノート
読み込み中…