Toluene → Ethyl 5-benzylamino-1-[3,5-difluoro-6-(p-methoxybenzylamino)pyridin-2-yl]-6,7,8-trifluoro-4-oxo-1,4-dihydroquinoline-3-carboxylate

HRID 368501노트

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HRID 368501 반응식
C1(C)C=CC=CC=1.[F:8][C:9]1[C:10]([N:26]2[C:35]3[C:30](=[C:31](F)[C:32]([F:38])=[C:33]([F:37])[C:34]=3[F:36])[C:29](=[O:40])[C:28]([C:41]([O:43][CH2:44][CH3:45])=[O:42])=[CH:27]2)=[N:11][C:12]([NH:16][CH2:17][C:18]2[CH:23]=[CH:22][C:21]([O:24][CH3:25])=[CH:20][CH:19]=2)=[C:13]([F:15])[CH:14]=1.[CH2:46]([NH2:53])[C:47]1[CH:52]=[CH:51][CH:50]=[CH:49][CH:48]=1>CCCCCC>[CH2:46]([NH:53][C:31]1[C:32]([F:38])=[C:33]([F:37])[C:34]([F:36])=[C:35]2[C:30]=1[C:29](=[O:40])[C:28]([C:41]([O:43][CH2:44][CH3:45])=[O:42])=[CH:27][N:26]2[C:10]1[C:9]([F:8])=[CH:14][C:13]([F:15])=[C:12]([NH:16][CH2:17][C:18]2[CH:23]=[CH:22][C:21]([O:24][CH3:25])=[CH:20][CH:19]=2)[N:11]=1)[C:47]1[CH:52]=[CH:51][CH:50]=[CH:49][CH:48]=1

참가 물질

5

반응물 3

HCID 1140Toluene2회HCID 7504BenzylamineHCID 22121224Ethyl 1-[3,5-difluoro-6-(p-methoxybenzylamino)pyridin-2-yl]-5,6,7,8-tetrafluoro-4-oxo-1,4-dihydroquinoline-3-carboxylate

생성물 1

HCID 22121197Ethyl 5-benzylamino-1-[3,5-difluoro-6-(p-methoxybenzylamino)pyridin-2-yl]-6,7,8-trifluoro-4-oxo-1,4-dihydroquinoline-3-carboxylate수율 65.4%

시약·촉매·용매 1

HCID 8058Hexane용매

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온도
110 °C

실험 절차

To 8 ml of toluene were added 1.58 g of ethyl 1-[3,5-difluoro-6-(p-methoxybenzylamino)pyridine-2-yl]-5,6,7,8-tetrafluoro-4-oxo-1,4-dihydroquinoline-3-carboxylate together with 0.68 g of benzylamine, and the mixture was stirred at 110° C. for 20 minutes and allowed to cool. After adding 15 ml of toluene and 15 ml of n-hexane, the mixture was washed twice with 300 ml of distilled water. The organic layer was dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. To the residue was added 4 ml of ethanol, and the solution was allowed to stand, and the precipitate was collected by filtration and washed with ethanol to obtain 1.20 g of the title compound as a yellow powder.

후처리

  1. temperatureto cool
  2. washthe mixture was washed twice with 300 ml of distilled water
  3. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. additionTo the residue was added 4 ml of ethanol
  6. filtrationthe precipitate was collected by filtration
  7. washwashed with ethanol

출처 및 근거

ORD 기록
ord-c5cc779034804bdab6ac6becf502a3b8
출처 데이터셋
uspto-grants-2000_10
특허 번호
US06133284

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