Ethanol → Garenoxacin Mesylate

HRID 1018534노트

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HRID 1018534 반응식
C([OH:3])C.[CH:4]1([N:7]2[C:16]3[C:11](=[CH:12][CH:13]=[C:14]([C:21]4[CH:22]=[C:23]5[C:27](=[CH:28][CH:29]=4)[C@@H:26]([CH3:30])[NH:25][CH2:24]5)[C:15]=3[O:17][CH:18]([F:20])[F:19])[C:10](=[O:31])[C:9]([C:32]([OH:34])=[O:33])=[CH:8]2)[CH2:6][CH2:5]1.[CH3:35][S:36]([OH:39])(=[O:38])=[O:37]>O>[OH2:3].[CH3:35][S:36]([OH:39])(=[O:38])=[O:37].[CH:4]1([N:7]2[C:16]3[C:11](=[CH:12][CH:13]=[C:14]([C:21]4[CH:22]=[C:23]5[C:27](=[CH:28][CH:29]=4)[C@@H:26]([CH3:30])[NH:25][CH2:24]5)[C:15]=3[O:17][CH:18]([F:20])[F:19])[C:10](=[O:31])[C:9]([C:32]([OH:34])=[O:33])=[CH:8]2)[CH2:6][CH2:5]1

참가 물질

5

반응물 3

HCID 702EthanolHCID 6395Methanesulfonic AcidHCID 124093Garenoxacin

생성물 1

HCID 157690Garenoxacin Mesylate

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
40 °C

실험 절차

In 192 ml of 50% water-containing ethanol is suspended 24 g of (R)-1-cyclopropyl-8-difluoromethoxy-7-(1-methyl-2,3-dihydro-1H-5-isoindolyl)-4-oxo-1,4-dihydro-3-quinolinecarboxylic acid and the suspension is warmed to 40° C., after which 5.71 g of methanesulfonic acid is added to the warmed suspension to form a uniform solution. Subsequently, the solution is stirred at the same temperature for 10 minutes and thereafter filtered, and the filtrate is concentrated, after which the crystals deposited are collected by filtration to obtain 26.64 g of (R)-1-cyclopropyl-8-difluoromethoxy-7-(1-methyl-2,3-dihydro-1H-5-isoindolyl)-4-oxo-1,4-dihydro-3-quinolinecarboxylic acid methanesulfonate monohydrate.

후처리

  1. customto form a uniform solution
  2. filtrationfiltered
  3. concentrationthe filtrate is concentrated
  4. filtrationafter which the crystals deposited are collected by filtration

출처 및 근거

ORD 기록
ord-a1d75f703c4e423ea26e59fa15d2f188
출처 데이터셋
uspto-grants-2002_11
특허 번호
US06482835B2

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