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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
ノート
印刷プレビュー

反応式

HRID 369285 の反応式
[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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

反応条件

温度
40 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8c4420c2d4d742018160f6f143d7d67c
出典データセット
uspto-grants-2000_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06136823

反応ノート

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