반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH3:14])[N:9]=[CH:8][CH:7]=[C:6]2[S:15][C:16]1[CH:24]=[CH:23][C:22]([F:25])=[CH:21][C:17]=1[C:18]([OH:20])=[O:19].S(Cl)(Cl)=O.[CH2:30](O)[CH3:31]>>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH3:14])[N:9]=[CH:8][CH:7]=[C:6]2[S:15][C:16]1[CH:24]=[CH:23][C:22]([F:25])=[CH:21][C:17]=1[C:18]([O:20][CH2:30][CH3:31])=[O:19]참가 물질
반응 조건
- 온도
- 0 °C
실험 절차
2-(6,7-Dimethoxy-quinolin-4-ylsulfanyl)-5-fluoro-benzoic acid (76 mg) was suspended in ethanol (387 mg), and the suspension was cooled at 0° C. Thionyl chloride (50 mg) was gradually added dropwise thereto, and the mixture was then heated under reflux for 20 min. The solvent was removed by distillation under the reduced pressure, water was added to the residue, and the mixture was neutralized with a 20% aqueous sodium hydroxide solution and was then extracted with ethyl acetate. Next, the ethyl acetate layer was washed with water and saturated brine and was dried over anhydrous sodium sulfate. The solvent was removed by distillation under the reduced pressure, and the residue was purified by column chromatography using acetone-hexane to give the title compound (68 mg, 84%).
후처리
- temperaturethe mixture was then heated
- temperatureunder reflux for 20 min
- customThe solvent was removed by distillation under the reduced pressure, water
- additionwas added to the residue
- extractionwas then extracted with ethyl acetate
- washNext, the ethyl acetate layer was washed with water and saturated brine
- dry with materialwas dried over anhydrous sodium sulfate
- customThe solvent was removed by distillation under the reduced pressure
- customthe residue was purified by column chromatography
출처 및 근거
- ORD 기록
- ord-ab1cd4f2ce044492810a09c0dc77ac37
- 출처 데이터셋
- uspto-grants-2009_07
- 특허 번호
- US07560558B2
연결된 노트
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