반응식
[CH2:1]([NH:3][CH:4]1[CH2:7][NH:6][CH2:5]1)[CH3:2].[NH2:8][C:9]1[N:14]=[C:13]([N:15]2[C:24]3[C:19](=[CH:20][C:21]([F:27])=[C:22](F)[C:23]=3[Br:25])[C:18](=[O:28])[C:17]([C:29]([OH:31])=[O:30])=[CH:16]2)[C:12]([F:32])=[CH:11][C:10]=1[F:33].CN1CCCC1.C(OC(C)C)(C)C>CS(C)=O>[NH2:8][C:9]1[N:14]=[C:13]([N:15]2[C:24]3[C:19](=[CH:20][C:21]([F:27])=[C:22]([N:6]4[CH2:7][CH:4]([NH:3][CH2:1][CH3:2])[CH2:5]4)[C:23]=3[Br:25])[C:18](=[O:28])[C:17]([C:29]([OH:31])=[O:30])=[CH:16]2)[C:12]([F:32])=[CH:11][C:10]=1[F:33]참가 물질
6
반응물 4
생성물 1
시약·촉매·용매 1
반응 조건
- 온도
- 40 °C
실험 절차
3-Ethylaminoazetidine (700 mg), 1-(6-amino-3,5-difluoropyridin-2-yl)-8-bromo-6,7-difluoro-4-oxo-1,4-dihydroquinoline-3-carboxylic acid (1.5 g), N-methyl-pyrrolidine (2.0 g)and dimethylsulfoxide (4.5 g) were combined, and the mixture was heated under stirring at 40° C. for 24 hours. After the mixture was allowed to cool down, isopropyl ether (10 mL) was added, the mixture was stirred, and a clear layer at the top of the mixture was removed. The same procedure was repeated once more, and the residue was concentrated under reduced pressure. Ethanol (5 mL) was added, and the mixture was heated under stirring at 70° C. for 30 minutes. The precipitated solid was collected by filtration. The title compound (1.38 g) was obtained.
후처리
- temperaturethe mixture was heated
- temperatureto cool down
- stirringthe mixture was stirred
- customa clear layer at the top of the mixture was removed
- concentrationthe residue was concentrated under reduced pressure
- additionEthanol (5 mL) was added
- temperaturethe mixture was heated
- stirringunder stirring at 70° C. for 30 minutes
- filtrationThe precipitated solid was collected by filtration
출처 및 근거
- ORD 기록
- ord-f1b6525d2c034223888dbf7e1495eaa4
- 출처 데이터셋
- uspto-grants-2005_02
- 특허 번호
- US06858625B1
연결된 노트
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