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Methylamine → 1-(5-Amino-2,4-difluorophenyl)-6-fluoro-5,8-dimethyl-7-methylamino-4-oxo-1,4-dihydroquinoline-3-carboxylic Acid

HRID 369285
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HRID 369285 반응식
[CH3:1][NH2:2].[NH2:3][C:4]1[C:5]([F:29])=[CH:6][C:7]([F:28])=[C:8]([N:10]2[C:19]3[C:14](=[C:15]([CH3:23])[C:16]([F:22])=[C:17](F)[C:18]=3[CH3:20])[C:13](=[O:24])[C:12]([C:25]([OH:27])=[O:26])=[CH:11]2)[CH:9]=1>N1C=CC=CC=1>[NH2:3][C:4]1[C:5]([F:29])=[CH:6][C:7]([F:28])=[C:8]([N:10]2[C:19]3[C:14](=[C:15]([CH3:23])[C:16]([F:22])=[C:17]([NH:2][CH3:1])[C:18]=3[CH3:20])[C:13](=[O:24])[C:12]([C:25]([OH:27])=[O:26])=[CH:11]2)[CH:9]=1
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참가 물질

4

반응물 2

HCID 6329MethylamineHCID 155184811-(3-amino-4,6-difluorophenyl)-6,7-difluoro-5,8-dimethyl-4-oxo-1,4-dihydroquinoline-3-carboxylic Acid

생성물 1

HCID 232847851-(5-Amino-2,4-difluorophenyl)-6-fluoro-5,8-dimethyl-7-methylamino-4-oxo-1,4-dihydroquinoline-3-carboxylic Acid

시약·촉매·용매 1

HCID 1049Pyridine용매

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온도
40 °C

실험 절차

Pyridine (300 mg) and a 40% aqueous solution (150 mg) of methylamine were added to 1-(5-amino-2,4-difluorophenyl)-6,7-difluoro-5,8-dimethyl-4-oxo-1,4-dihydroquinoline-3-carboxylic acid (110 mg), and the mixture was heated and stirred at 40° C. for 8 days. The solvent and the like were distilled off under reduced pressure, and ethanol (0.5 ml) was added to the residue. The mixture was left to stand for 3 days, and solids deposited were collected by filtration and washed with ethanol and diethyl ether to obtain the title compound (20 mg) as a pale yellow powder.

후처리

  1. temperaturethe mixture was heated
  2. distillationThe solvent and the like were distilled off under reduced pressure, and ethanol (0.5 ml)
  3. additionwas added to the residue
  4. waitThe mixture was left
  5. waitto stand for 3 days
  6. filtrationsolids deposited were collected by filtration
  7. washwashed with ethanol and diethyl ether

출처 및 근거

ORD 기록
ord-8c4420c2d4d742018160f6f143d7d67c
출처 데이터셋
uspto-grants-2000_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06136823

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