Ethanolamine → 1-(5-Amino-2,4-difluorophenyl)-8-chloro-6-fluoro-7-(2-hydroxyethylamino)-4-oxo-1,4-dihydroquinoline-3-carboxylic acid ethanolamine salt

HRID 369273ノート

反応式

HRID 369273 の反応式
[NH2:1][C:2]1[C:3]([F:26])=[CH:4][C:5]([F:25])=[C:6]([N:8]2[C:17]3[C:12](=[CH:13][C:14]([F:20])=[C:15](F)[C:16]=3[Cl:18])[C:11](=[O:21])[C:10]([C:22]([OH:24])=[O:23])=[CH:9]2)[CH:7]=1.[CH2:27]([CH2:29][NH2:30])[OH:28]>N1C=CC=CC=1>[CH2:27]([CH2:29][NH2:30])[OH:28].[NH2:1][C:2]1[C:3]([F:26])=[CH:4][C:5]([F:25])=[C:6]([N:8]2[C:17]3[C:12](=[CH:13][C:14]([F:20])=[C:15]([NH:30][CH2:29][CH2:27][OH:28])[C:16]=3[Cl:18])[C:11](=[O:21])[C:10]([C:22]([OH:24])=[O:23])=[CH:9]2)[CH:7]=1

参加物

4

反応物 2

HCID 700EthanolamineHCID 108619991-(3-Amino-4,6-difluorophenyl)-8-chloro-6,7-difluoro-1,4-dihydro-4-oxoquinoline-3-carboxylic acid

生成物 1

HCID 699596811-(5-Amino-2,4-difluorophenyl)-8-chloro-6-fluoro-7-(2-hydroxyethylamino)-4-oxo-1,4-dihydroquinoline-3-carboxylic acid ethanolamine salt収率 79.5%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

反応条件

温度
50 °C

実験手順

1-(5-Amino-2,4-difluorophenyl)-8-chloro-6,7-difluoro-4-oxo-1,4-dihydroquinoline-3-carboxylic acid (600 mg) and ethanolamine (600 mg) were added to pyridine (2,500 mg), and the mixture was stirred at 50° C. for 1.5 hours. The reaction mixture was concentrated under reduced pressure, and ethanol (6 ml) was added to the residue. Deposits were collected by filtration and washed with ethanol and diisopropyl ether in that order to obtain the title compound (603 mg) as a colorless powder.

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure, and ethanol (6 ml)
  2. additionwas added to the residue
  3. filtrationDeposits were collected by filtration
  4. washwashed with ethanol and diisopropyl ether in that order

出典と根拠

ORDレコード
ord-3ef117c1da7c4dad8fdef301fafffebc
出典データセット
uspto-grants-2000_10
特許番号
US06136823

反応ノート

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