Methanesulfonic Acid → 1-Cyclopropyl-8-difluoromethoxy-6-fluoro-7-(3-methylpiperazinyl)-1,4-dihydro-4-oxoquinoline-3-carboxylic acid methanesulfonic acid salt

HRID 1440120노트

반응식

HRID 1440120 반응식
[CH3:1][S:2]([OH:5])(=[O:4])=[O:3].[CH:6]1([N:9]2[C:18]3[C:13](=[CH:14][C:15]([F:30])=[C:16]([N:23]4[CH2:28][CH2:27][NH:26][CH:25]([CH3:29])[CH2:24]4)[C:17]=3[O:19][CH:20]([F:22])[F:21])[C:12](=[O:31])[C:11]([C:32]([OH:34])=[O:33])=[CH:10]2)[CH2:8][CH2:7]1>CO>[CH3:1][S:2]([OH:5])(=[O:4])=[O:3].[CH:6]1([N:9]2[C:18]3[C:13](=[CH:14][C:15]([F:30])=[C:16]([N:23]4[CH2:28][CH2:27][NH:26][CH:25]([CH3:29])[CH2:24]4)[C:17]=3[O:19][CH:20]([F:22])[F:21])[C:12](=[O:31])[C:11]([C:32]([OH:34])=[O:33])=[CH:10]2)[CH2:8][CH2:7]1

참가 물질

4

반응물 2

HCID 6395Methanesulfonic AcidHCID 150237881-Cyclopropyl-8-difluoromethoxy-6-fluoro-7-(3-methylpiperazinyl)-1,4-dihydro-4-oxoquinoline-3-carboxylic acid

생성물 1

HCID 867452961-Cyclopropyl-8-difluoromethoxy-6-fluoro-7-(3-methylpiperazinyl)-1,4-dihydro-4-oxoquinoline-3-carboxylic acid methanesulfonic acid salt수율 95.5%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

0.093 g (0.00097 moles) of methanesulfonic acid was added to a suspension of 0.40 g of 1-cyclopropyl-8-difluoromethoxy-6-fluoro-7-(3-methylpiperazinyl)-1,4-dihydro-4-oxoquinoline-3-carboxylic acid (prepared as described in Example 1) in 50 ml of methanol to obtain a transparent solution. This was concentrated by evaporation under reduced pressure, and the residue was washed with ethanol, to give 0.47 g of the title compound (methanesulfonic acid salt) as a colorless powder, melting at 289°-292° C. (with decomposition).

후처리

  1. customto obtain a transparent solution
  2. concentrationThis was concentrated by evaporation under reduced pressure
  3. washthe residue was washed with ethanol

출처 및 근거

ORD 기록
ord-9dc1aefc113d4572b572ea3d082a314a
출처 데이터셋
uspto-grants-1996_03
특허 번호
US05496951

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