Methanesulfonic Acid → Garenoxacin Mesylate

HRID 1250358노트

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HRID 1250358 반응식
O.[CH:2]1([N:5]2[C:14]3[C:9](=[CH:10][CH:11]=[C:12]([C:19]4[CH:20]=[C:21]5[C:25](=[CH:26][CH:27]=4)[C@@H:24]([CH3:28])[NH:23][CH2:22]5)[C:13]=3[O:15][CH:16]([F:18])[F:17])[C:8](=[O:29])[C:7]([C:30]([OH:32])=[O:31])=[CH:6]2)[CH2:4][CH2:3]1.[CH3:33][S:34]([OH:37])(=[O:36])=[O:35]>C(O)C>[OH2:15].[CH3:33][S:34]([OH:37])(=[O:36])=[O:35].[CH:2]1([N:5]2[C:14]3[C:9](=[CH:10][CH:11]=[C:12]([C:19]4[CH:20]=[C:21]5[C:25](=[CH:26][CH:27]=4)[C@@H:24]([CH3:28])[NH:23][CH2:22]5)[C:13]=3[O:15][CH:16]([F:18])[F:17])[C:8](=[O:29])[C:7]([C:30]([OH:32])=[O:31])=[CH:6]2)[CH2:4][CH2:3]1

참가 물질

4

반응물 2

HCID 6395Methanesulfonic AcidHCID 68432514HCID 68432514, 화합물

생성물 1

HCID 157690Garenoxacin Mesylate수율 182.5%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
40 °C

실험 절차

In 192 ml of 50% 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 monohydrate, and the suspension is warmed to 40° C., after which 5.71 g of methanesulfonic acid is added to form a uniform solution. Subsequently, 2.4 g of activated carbon is added and the resulting mixture is stirred at the same temperature for 10 minutes, after which the insolubles are removed by filtration. The filtrate is concentrated and 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. additionSubsequently, 2.4 g of activated carbon is added
  3. customafter which the insolubles are removed by filtration
  4. concentrationThe filtrate is concentrated
  5. filtrationthe crystals deposited are collected by filtration

출처 및 근거

ORD 기록
ord-53f26a2272544d19840de385007015a3
출처 데이터셋
uspto-grants-2002_01
특허 번호
US06337399B1

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