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Acetonitrile → 7-[(7S)-7-Amino-7-methylspiro[2.4]hept-5-yl]-1,4-dihydro-6-fluoro-1-[(1R,2S)-2-fluorocyclopropyl]-8-methoxy-4-oxo-3-quinolinecarboxylic acid dihydrate

HRID 254865
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HRID 254865 반응식
[C:1](#N)C.[F:4][C:5]1[CH:6]=[C:7]2[C:12](=[C:13]([O:16][CH3:17])[C:14]=1F)[N:11]([C@@H:18]1[CH2:20][C@@H:19]1[F:21])[CH:10]=[C:9]([C:22]([OH:24])=[O:23])[C:8]2=[O:25].Cl.Cl.C([CH:35]1[C:37]2([C@:41]([CH3:43])([NH2:42])[CH2:40]N[CH2:38]2)[CH2:36]1)C1C=CC=CC=1>C(N(CC)CC)C>[OH2:16].[OH2:16].[NH2:42][C@:41]1([CH3:43])[C:37]2([CH2:36][CH2:35]2)[CH2:38][CH:1]([C:14]2[C:13]([O:16][CH3:17])=[C:12]3[C:7]([C:8](=[O:25])[C:9]([C:22]([OH:24])=[O:23])=[CH:10][N:11]3[C@@H:18]3[CH2:20][C@@H:19]3[F:21])=[CH:6][C:5]=2[F:4])[CH2:40]1
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참가 물질

5

반응물 3

HCID 6342AcetonitrileHCID 120946186,7-difluoro-1,4-dihydro-1-[(1R,2S)-2-fluorocyclopropyl]-8-methoxy-4-oxo-3-quinolinecarboxylic acidHCID 66700197benzyl-(7S)-7-methyl-5-azaspiro[2.4]heptan-7-amine dihydrochloride

생성물 1

HCID 667002067-[(7S)-7-Amino-7-methylspiro[2.4]hept-5-yl]-1,4-dihydro-6-fluoro-1-[(1R,2S)-2-fluorocyclopropyl]-8-methoxy-4-oxo-3-quinolinecarboxylic acid dihydrate수율 91%

시약·촉매·용매

1
HCID 8471Triethylamine용매2회

실험 절차

An acetonitrile solution (800 mL) containing 6,7-difluoro-1,4-dihydro-1-[(1R,2S)-2-fluorocyclopropyl]-8-methoxy-4-oxo-3-quinolinecarboxylic acid (90 g), benzyl-(7S)-7-methyl-5-azaspiro[2.4]heptan-7-amine dihydrochloride (90 g), triethylamine (39.9 mL), and boron trifluoride-tetrahydrofuran complex (63.4 mL) was stirred at room temperature for 30 minutes. Boron trifluoride-tetrahydrofuran complex (6.3 mL) was further added to the solution, followed by stirring for one hour at the same temperature. Triethylamine (159.5 mL) was further added to the reaction mixture, followed by stirring at room temperature for 16 hours. The solvent was evaporated under reduced pressure, and methanol (900 mL) was added to the residue. The mixture was refluxed for 6 hours. After cooling to room temperature, the mixture was stirred at 40° C. for 5 hours under hydrogen in the presence of 5% Pd—C (4.5 g). Subsequently, triethylamine (90 mL) and water (225 mL) were added to the thus-obtained reaction mixture, followed by stirring at 40° C. for one hour. Pd—C was removed through filtration, and the filtrate was concentrated under reduced pressure. Water (720 mL) and methanol (180 mL) were added to the residue, and the pH of the product was adjusted to 8 by use of 5N aqueous sodium hydroxide solution. The thus-obtained mixture was stirred at 60° C. for 40 minutes, and the pH of the product was adjusted to 7 by use of 5N aqueous sodium hydroxide solution, followed by stirring at room temperature for one hour. The thus-produced crystals were recovered through filtration and dried, to thereby yield 120.9 g of the title compound as pale brown crystals (yield: 91%).

후처리

  1. additionBoron trifluoride-tetrahydrofuran complex (6.3 mL) was further added to the solution
  2. stirringby stirring for one hour at the same temperature
  3. stirringby stirring at room temperature for 16 hours
  4. customThe solvent was evaporated under reduced pressure, and methanol (900 mL)
  5. additionwas added to the residue
  6. temperatureThe mixture was refluxed for 6 hours
  7. temperatureAfter cooling to room temperature
  8. stirringthe mixture was stirred at 40° C. for 5 hours under hydrogen in the presence of 5% Pd—C (4.5 g)
  9. additionSubsequently, triethylamine (90 mL) and water (225 mL) were added to the thus-obtained reaction mixture
  10. stirringby stirring at 40° C. for one hour
  11. customPd—C was removed through filtration
  12. concentrationthe filtrate was concentrated under reduced pressure
  13. additionWater (720 mL) and methanol (180 mL) were added to the residue
  14. stirringThe thus-obtained mixture was stirred at 60° C. for 40 minutes
  15. stirringby stirring at room temperature for one hour
  16. filtrationThe thus-produced crystals were recovered through filtration
  17. customdried

출처 및 근거

ORD 기록
ord-a6168cd098ca40e3abd3ac26e35aed1a
출처 데이터셋
uspto-grants-2011_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07875722B2

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