4,7-Dichloro-8-nitroquinoline → 7-Chloro-4-methoxy-8-nitro-quinoline
反応式
[CH3:1][O-:2].[Na+].Cl[C:5]1[C:14]2[C:9](=[C:10]([N+:16]([O-:18])=[O:17])[C:11]([Cl:15])=[CH:12][CH:13]=2)[N:8]=[CH:7][CH:6]=1>CO>[Cl:15][C:11]1[C:10]([N+:16]([O-:18])=[O:17])=[C:9]2[C:14]([C:5]([O:2][CH3:1])=[CH:6][CH:7]=[N:8]2)=[CH:13][CH:12]=1参加物
4
実験手順
Sodium methoxide (2.0 g, 37.0 mmol) was added to a solution of 4,7-dichloro-8-nitro-quinoline (Intermediate 68) (3.0 g, 12.3 mmol) in MeOH (20 ml) and the reaction was heated under reflux for 24 h. The solvent was removed in vacuo. The residue was dissolved in EtOAc (150 ml) and washed with water, dried (MgSO4) and concentrated in vacuo. The crude residue was purified by column chromatography with EtOAc/heptane (4:1) to give the title compound (2.54 g, 83%).
後処理
- temperaturethe reaction was heated
- temperatureunder reflux for 24 h
- customThe solvent was removed in vacuo
- dissolutionThe residue was dissolved in EtOAc (150 ml)
- washwashed with water
- dry with materialdried (MgSO4)
- concentrationconcentrated in vacuo
- customThe crude residue was purified by column chromatography with EtOAc/heptane (4:1)
出典と根拠
- ORDレコード
- ord-5e2519145ddf45159096887159a6f22f
- 出典データセット
- uspto-grants-2015_08
- 特許番号
- US09102688B2
反応ノート
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