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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Piperazine → 6-Fluoro-1-(2,4-difluorophenyl)-1,4-dihydro-5-methyl-4-oxo-7-(1-piperazinyl)-3-quinolinecarboxylic acid

HRID 2073855
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HRID 2073855 반응식
[F:1][C:2]1[C:3]([CH3:27])=[C:4]2[C:9](=[CH:10][C:11]=1F)[N:8]([C:13]1[CH:18]=[CH:17][C:16]([F:19])=[CH:15][C:14]=1[F:20])[CH:7]=[C:6]([C:21]([O:23]CC)=[O:22])[C:5]2=[O:26].[NH:28]1[CH2:33][CH2:32][NH:31][CH2:30][CH2:29]1>C(#N)C>[F:1][C:2]1[C:3]([CH3:27])=[C:4]2[C:9](=[CH:10][C:11]=1[N:28]1[CH2:33][CH2:32][NH:31][CH2:30][CH2:29]1)[N:8]([C:13]1[CH:18]=[CH:17][C:16]([F:19])=[CH:15][C:14]=1[F:20])[CH:7]=[C:6]([C:21]([OH:23])=[O:22])[C:5]2=[O:26]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 4837PiperazineHCID 14774107Ethyl 1-(2,4-difluorophenyl)-5-methyl-6,7-difluoro-1,4-dihydro-4-oxoquinoline-3-carboxylate

생성물 1

HCID 146512396-Fluoro-1-(2,4-difluorophenyl)-1,4-dihydro-5-methyl-4-oxo-7-(1-piperazinyl)-3-quinolinecarboxylic acid수율 69.5%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A solution of 0.76 g (2.00 mmol) of ethyl 6,7-difluoro-1-(2,4-difluorophenyl)-1,4-dihydro-5-methyl-4-oxo-3-quinolinecarboxylate, 0.69 g (8.00 mmol) of anhydrous piperazine, and 30 ml of acetonitrile was refluxed for 18 hours, cooled, and concentrated. The residue was dissolved in 20 ml 6N hydrochloric acid and refluxed for three hours. The suspension was cooled, concentrated by half and filtered, and the solids were washed with water. The crude product was suspended in water which was made basic (pH 12), filtered, and neutralized to pH 6.8. The precipitate was filtered and neutralized to pH 6.8. The precipitate was filtered, washed with water, and dried to give 0.58 g of the title compound, mp 198°-200° C.

후처리

  1. temperaturecooled
  2. concentrationconcentrated
  3. dissolutionThe residue was dissolved in 20 ml 6N hydrochloric acid
  4. temperaturerefluxed for three hours
  5. temperatureThe suspension was cooled
  6. concentrationconcentrated by half
  7. filtrationfiltered
  8. washthe solids were washed with water
  9. filtrationfiltered
  10. filtrationThe precipitate was filtered
  11. filtrationThe precipitate was filtered
  12. washwashed with water
  13. customdried

출처 및 근거

ORD 기록
ord-690c95b8a0964bb9ab1cafdd98ecfa8b
출처 데이터셋
uspto-grants-1990_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04920120

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