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Piperazine → Methyl 1-ethyl-6-fluoro-4-oxo-7-piperazin-1-ylquinoline-3-carboxylate

HRID 2418468
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인쇄 미리보기

반응식

HRID 2418468 반응식
[NH:1]1[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.[CH3:7][O:8][C:9]([C:11]1[C:20](=[O:21])[C:19]2[C:14](=[CH:15][C:16](Cl)=[C:17]([F:22])[CH:18]=2)[N:13]([CH2:24][CH3:25])[CH:12]=1)=[O:10]>N1C=CC=CC=1>[CH3:7][O:8][C:9]([C:11]1[C:20](=[O:21])[C:19]2[C:14](=[CH:15][C:16]([N:1]3[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]3)=[C:17]([F:22])[CH:18]=2)[N:13]([CH2:24][CH3:25])[CH:12]=1)=[O:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 4837PiperazineHCID 12079768HCID 12079768, 화합물

생성물 1

HCID 12733940Methyl 1-ethyl-6-fluoro-4-oxo-7-piperazin-1-ylquinoline-3-carboxylate수율 94.2%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

A mixture of 1.7 g of anhydrous piperazine and 1.4 g of 1-ethyl-6-fluoro-7-chloro-4-oxo-1,4-dihydroquinoline-3-carboxylic acid methyl ester in 3 ml of pyridine was refluxed with stirring for 5 hrs. The reaction mixture was cooled to give crude crystals. The crude crystals were recrystallized from a mixture of methylene chloride and methanol to give 1.55 g (77.5% yield) of 1-ethyl-6-fluoro-7-(1-piperazinyl)-4-oxo-1,4-dihydroquinoline-3-carboxylic acid methyl ester. mp: 179°-181° C.

후처리

  1. temperaturewas refluxed
  2. temperatureThe reaction mixture was cooled
  3. customto give crude crystals
  4. customThe crude crystals were recrystallized from a mixture of methylene chloride and methanol

출처 및 근거

ORD 기록
ord-d645f4d403694c0094beca61b89d8f5c
출처 데이터셋
uspto-grants-1984_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04472579

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