반응식
[CH2:1]([N:3]1[C:12]2[C:7](=[CH:8][C:9]([F:24])=[C:10]([N:14]3[CH2:19][CH2:18][O:17][CH:16]([CH2:20][NH:21]C=O)[CH2:15]3)[C:11]=2[F:13])[C:6](=[O:25])[C:5]([C:26]([OH:28])=[O:27])=[CH:4]1)[CH3:2].[ClH:29].O>CO>[ClH:29].[NH2:21][CH2:20][CH:16]1[CH2:15][N:14]([C:10]2[C:11]([F:13])=[C:12]3[C:7]([C:6](=[O:25])[C:5]([C:26]([OH:28])=[O:27])=[CH:4][N:3]3[CH2:1][CH3:2])=[CH:8][C:9]=2[F:24])[CH2:19][CH2:18][O:17]1참가 물질
5
실험 절차
A solution of 500 mg of 1-ethyl-6,8-difluoro-7-[2-(formylaminomethyl)morpholino]-1,4-dihydro-4-oxoquinoline-3-carboxylic acid, 1 ml of concentrated hydrochloric acid, 2 ml of water and 10 ml of methanol is refluxed for 1.5 hours. The reaction mixture is concentrated under reduced pressure. The obtained crystals are washed with acetone, collected by filtration and recrystallized from dimethylformamide to give 7-[2-(aminomethyl)morpholino]-1-ethyl-6,8-difluoro-1,4-dihydro-4-oxoquinoline-3-carboxylic acid hydrochloride, melting at 276°-278° C. with decomposition.
후처리
- concentrationThe reaction mixture is concentrated under reduced pressure
- washThe obtained crystals are washed with acetone
- filtrationcollected by filtration
- customrecrystallized from dimethylformamide
출처 및 근거
- ORD 기록
- ord-1875382aeec84616b2a292f5272f54b6
- 출처 데이터셋
- uspto-grants-1989_12
- 특허 번호
- US04889857
연결된 노트
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