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Hydrochloric Acid → 7-(4-Acetyl-1-piperazinyl)-1-cyclopropyl-6, 8-difluoro-5-methyl-1,4-dihydro-4-oxoquinoline-3-carboxylic acid

HRID 2396985
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HRID 2396985 반응식
[N:1]1([C:7]2[C:16]([F:17])=[C:15]3[C:10]([C:11](=[O:24])[C:12]([C:21]([OH:23])=[O:22])=[CH:13][N:14]3[CH:18]3[CH2:20][CH2:19]3)=[C:9]([CH3:25])[C:8]=2[F:26])[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.[C:27](OC(=O)C)(=[O:29])[CH3:28].Cl>[OH-].[Na+]>[C:27]([N:4]1[CH2:5][CH2:6][N:1]([C:7]2[C:16]([F:17])=[C:15]3[C:10]([C:11](=[O:24])[C:12]([C:21]([OH:23])=[O:22])=[CH:13][N:14]3[CH:18]3[CH2:19][CH2:20]3)=[C:9]([CH3:25])[C:8]=2[F:26])[CH2:2][CH2:3]1)(=[O:29])[CH3:28]
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참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 7918Acetic AnhydrideHCID 146511701-Cyclopropyl-6,8-difluoro-1,4-dihydro-5-methyl-4-oxo-7-(1-piperazinyl)-3-quinolinecarboxylic acid

생성물 1

HCID 146512097-(4-Acetyl-1-piperazinyl)-1-cyclopropyl-6, 8-difluoro-5-methyl-1,4-dihydro-4-oxoquinoline-3-carboxylic acid

시약·촉매·용매 1

HCID 14798Sodium Hydroxide
용매

실험 절차

To a solution of 7-(1-piperazinyl)-1-cyclopropyl-6,8-difluoro-5-methyl-1, 4-dihydro-4-oxoquinoline-3carboxylic acid (42 mg) in 5% sodium hydroxide (2 ml) is added acetic anhydride (0.1 ml) at room temperature. After the mixture is made acidic with dilute hydrochloric acid, the resultant is extracted with dichloromethane and the extract is dried over magnesium sulfate. After concentrating, the obtained residue is recrystallized from ethanol to give 7-(4-acetyl-1-piperazinyl)-1-cyclopropyl-6,8-difluoro-5-methyl-1, 4-dihydro-4-oxoquinoline-3-carboxylic acid (30 mg), as white powder, m.p. 217°-220° C.

후처리

  1. extractionthe resultant is extracted with dichloromethane
  2. dry with materialthe extract is dried over magnesium sulfate
  3. concentrationAfter concentrating
  4. customthe obtained residue is recrystallized from ethanol

출처 및 근거

ORD 기록
ord-428eefedaf084867951dfa74d1813444
출처 데이터셋
uspto-grants-1996_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05495020

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