Formaldehyde → 7-(3,4-Dimethyl-1-piperazinyl)-1-ethyl-6,8-difluoro-1,4-dihydro-4-oxoquinoline-3-carboxlic acid
반응식
[CH2:1]([N:3]1[C:12]2[C:7](=[CH:8][C:9]([F:21])=[C:10]([N:14]3[CH2:19][CH2:18][NH:17][CH:16]([CH3:20])[CH2:15]3)[C:11]=2[F:13])[C:6](=[O:22])[C:5]([C:23]([OH:25])=[O:24])=[CH:4]1)[CH3:2].[CH2:26]=O>C(O)=O>[CH3:20][CH:16]1[N:17]([CH3:26])[CH2:18][CH2:19][N:14]([C:10]2[C:11]([F:13])=[C:12]3[C:7]([C:6](=[O:22])[C:5]([C:23]([OH:25])=[O:24])=[CH:4][N:3]3[CH2:1][CH3:2])=[CH:8][C:9]=2[F:21])[CH2:15]1참가 물질
4
실험 절차
A mixture of 1.40 g of 1-ethyl-6,8-difluoro-1,4-dihydro-7-(3-methyl-1-piperazinyl)-4-oxoquinoline-3-carboxylic acid, 2.8 ml of 90% formic acid and 2.2 ml of 37% formalin was heated for 4 hours under reflux. The reaction mixture was evaporated and the residue was dissolved in water. The solution was neutralized with aqueous sodium bicarbonate. The precipitate was filtered and recrystallized from ethanol to give 0.32 g of the title compound as colorless needles, M.p. 211.5°-212° C.
후처리
- temperaturewas heated for 4 hours
- temperatureunder reflux
- customThe reaction mixture was evaporated
- dissolutionthe residue was dissolved in water
- filtrationThe precipitate was filtered
- customrecrystallized from ethanol
출처 및 근거
- ORD 기록
- ord-841b7245c77b43c88fd1851b8beb19af
- 출처 데이터셋
- uspto-grants-1985_07
- 특허 번호
- US04528287
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