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

HRID 369256ノート

反応式

HRID 369256 の反応式
[NH2:1][C:2]1[N:7]=[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:5]=[CH:4][C:3]=1[F:25].[CH3:26][NH2:27]>N1C=CC=CC=1>[NH2:1][C:2]1[N:7]=[C:6]([N:8]2[C:17]3[C:12](=[CH:13][C:14]([F:20])=[C:15]([NH:27][CH3:26])[C:16]=3[Cl:18])[C:11](=[O:21])[C:10]([C:22]([OH:24])=[O:23])=[CH:9]2)[CH:5]=[CH:4][C:3]=1[F:25]

参加物

4

反応物 2

HCID 6329MethylamineHCID 221212661-(6-Amino-5-fluoropyridin-2-yl)-8-chloro-6,7-difluoro-4-oxo-1,4-dihydroquinoline-3-carboxylic acid

生成物 1

HCID 232847721-(6-Amino-5-fluoropyridin-2-yl)-8-chloro-6-fluoro-7-methylamino-4-oxo-1,4-dihydroquinoline-3-carboxylic Acid収率 103.2%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

1-(6-Amino-5-fluoropyridin-2-yl)-8-chloro-6,7-difluoro-4-oxo-1,4-dihydroquinoline-3-carboxylic acid (158 mg) and an aqueous solution (about 40%; 165 mg) of methylamine were added to pyridine (480 mg), and the mixture was stirred at room temperature for 17 hours. The reaction mixture was concentrated under reduced pressure, and ethanol (1 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 (168 mg) as a pale yellow powder.

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure, and ethanol (1 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-5e73a7593842475787cc5903e1fddf99
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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