Ethanol → HCID 68433833, 화합물

HRID 1018542노트

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HRID 1018542 반응식
C(O)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.[S:35](=[O:39])(=[O:38])([OH:37])[OH:36]>O>[S:35]([OH:39])([OH:38])(=[O:37])=[O:36].[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 1118Sulfuric AcidHCID 124093Garenoxacin

생성물 1

HCID 68433833HCID 68433833, 화합물수율 55.3%

시약·촉매·용매 1

HCID 962Water용매

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온도
50 °C

실험 절차

In 10 ml of 50% water-containing ethanol is suspended 0.5 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 then warmed to 50° C., after which 0.12 g of sulfuric acid is added thereto to form a uniform solution. Subsequently, the solution is stirred at the same temperature for 10 minutes and then filtered. The filtrate is cooled to room temperature and thereafter the crystals deposited are collected by filtration to obtain 0.34 g of (R)-1-cyclopropyl-8-difluoromethoxy-7-(1-methyl-2,3-dihydro-1H-5-isoindolyl)-4-oxo-1,4-dihydro-3-quinolinecarboxylic acid sulfate.

후처리

  1. customto form a uniform solution
  2. filtrationfiltered
  3. temperatureThe filtrate is cooled to room temperature
  4. filtrationthe crystals deposited are collected by filtration

출처 및 근거

ORD 기록
ord-750b023080a4441b9560a408e230d34c
출처 데이터셋
uspto-grants-2002_11
특허 번호
US06482835B2

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