홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

5-amino-6,7,8-trifluoro-[(1R,2S)-2-fluorocyclopropyl]-1,4-dihydro-4-oxoquinoline-3-carboxylic acid → 5-Amino-7-[3-(1-amino-1-cyclopropyl)methylpyrrolidin-1-yl]-6,8-difluoro-1-[2-(S)-fluoro-1-(R)-cyclopropyl]-1,4-dihydro-4-oxoquinoline-3-carboxylic acid

HRID 1368072
노트
인쇄 미리보기

반응식

HRID 1368072 반응식
C(O[C:9]([N:11]1[CH2:15][CH2:14][CH:13]([CH2:16][C:17]2([NH:20]C(OC(C)(C)C)=O)[CH2:19][CH2:18]2)[CH2:12]1)=O)C1C=CC=CC=1.[H][H].[NH2:30][C:31]1[C:40]([F:41])=C(F)[C:38]([F:43])=[C:37]2[C:32]=1[C:33](=[O:51])[C:34]([C:48]([OH:50])=[O:49])=[CH:35][N:36]2[C@@H:44]1[CH2:46][C@@H:45]1[F:47]>CO.[Pd]>[NH2:30][C:31]1[C:40]([F:41])=[C:9]([N:11]2[CH2:15][CH2:14][CH:13]([CH2:16][C:17]3([NH2:20])[CH2:18][CH2:19]3)[CH2:12]2)[C:38]([F:43])=[C:37]2[C:32]=1[C:33](=[O:51])[C:34]([C:48]([OH:50])=[O:49])=[CH:35][N:36]2[C@@H:44]1[CH2:46][C@@H:45]1[F:47]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 155235655-amino-6,7,8-trifluoro-[(1R,2S)-2-fluorocyclopropyl]-1,4-dihydro-4-oxoquinoline-3-carboxylic acidHCID 226339261-Benzyloxycarbonyl-3-[1-(tert-butoxycarbonyl)amino-1-cyclopropyl]methylpyrrolidineHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 696884275-Amino-7-[3-(1-amino-1-cyclopropyl)methylpyrrolidin-1-yl]-6,8-difluoro-1-[2-(S)-fluoro-1-(R)-cyclopropyl]-1,4-dihydro-4-oxoquinoline-3-carboxylic acid수율 60.9%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

1-Benzyloxycarbonyl-3-[1-(tert-butoxycarbonyl)amino-1-cyclopropyl]methylpyrrolidine (originated from F3 of Reference Example 4; 100 mg, 0.267 mmol) was dissolved in anhydrous methanol (20 ml), and the solution was mixed with 10% palladium on carbon catalyst (water content 50%, 100 mg) and stirred at room temperature for 1 hour in an atmosphere of hydrogen under atmospheric pressure. After filtration of the reaction solution through celite, the resulting filtrate was concentrated under a reduced pressure. The thus obtained residue and triethylamine (2 ml) were added to dry acetonitrile (8 ml), and the mixture was further mixed with 5-amino-6,7,8-trifluoro-1-[2-(S)-fluoro-1-(R)-cyclopropyl]-1,4-dihydro-4-oxoquinoline-3-carboxylic acid (80 mg, 0.222 mmol) and heated under reflux for 16 hours. After cooling of the reaction solution, the thus precipitated crystals were collected by filtration, washed with acetonitrile, mixed with concentrated hydrochloric acid (10 ml) under ice-cooling and then stirred at room temperature for 5 minutes. This was mixed with distilled water (15 ml), and the thus obtained acidic aqueous solution was washed with dichloromethane (20 ml×2), adjusted to pH 11 with sodium hydroxide aqueous solution under ice-cooling and then washed with chloroform (20 ml). The resulting basic aqueous solution was adjusted to pH 7.4 with 1 N hydrochloric acid and extracted with chloroform (80 ml×4). After drying over anhydrous sodium sulfate, the solvent was evaporated under a reduced pressure. Thereafter, the resulting residue was purified by recrystallizing from ethanol-28% aqueous ammonia and then dried under a reduced pressure, thereby obtaining 59 mg (60.8%) of the title compound as yellow needle crystals.

후처리

  1. filtrationAfter filtration of the reaction solution through celite
  2. concentrationthe resulting filtrate was concentrated under a reduced pressure
  3. additionThe thus obtained residue and triethylamine (2 ml) were added to dry acetonitrile (8 ml)
  4. temperatureheated
  5. temperatureunder reflux for 16 hours
  6. temperatureAfter cooling of the reaction solution
  7. filtrationthe thus precipitated crystals were collected by filtration
  8. washwashed with acetonitrile
  9. additionmixed with concentrated hydrochloric acid (10 ml) under ice-
  10. temperaturecooling
  11. additionThis was mixed with distilled water (15 ml)
  12. washthe thus obtained acidic aqueous solution was washed with dichloromethane (20 ml×2)
  13. temperaturecooling
  14. washwashed with chloroform (20 ml)
  15. extractionextracted with chloroform (80 ml×4)
  16. dry with materialAfter drying over anhydrous sodium sulfate
  17. customthe solvent was evaporated under a reduced pressure
  18. customThereafter, the resulting residue was purified
  19. customby recrystallizing from ethanol-28% aqueous ammonia
  20. customdried under a reduced pressure

출처 및 근거

ORD 기록
ord-65685ce0ffba45c494b0d225d05243bd
출처 데이터셋
uspto-grants-2003_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06573260B1

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트