Hydrochloric Acid → 1-(4-Amino-5-fluoropyridin-2-yl)-8-chloro-6,7-difluoro-4-oxo-1,4-dihydroquinoline-3-carboxylic acid

HRID 610239ノート

反応式

HRID 610239 の反応式
Cl.[NH2:2][C:3]1[C:8]([F:9])=[CH:7][N:6]=[C:5]([N:10]2[C:19]3[C:14](=[CH:15][C:16]([F:22])=[C:17]([F:21])[C:18]=3[Cl:20])[C:13](=[O:23])[C:12]([C:24]([O:26]CC)=[O:25])=[CH:11]2)[CH:4]=1>C(O)(=O)C>[NH2:2][C:3]1[C:8]([F:9])=[CH:7][N:6]=[C:5]([N:10]2[C:19]3[C:14](=[CH:15][C:16]([F:22])=[C:17]([F:21])[C:18]=3[Cl:20])[C:13](=[O:23])[C:12]([C:24]([OH:26])=[O:25])=[CH:11]2)[CH:4]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 22121193Ethyl 1-(4-amino-5-fluoropyridine-2-yl)-8-chloro-6,7-difluoro-4-oxo-1,4-dihydroquinoline-3-carboxylate

生成物 1

HCID 221211881-(4-Amino-5-fluoropyridin-2-yl)-8-chloro-6,7-difluoro-4-oxo-1,4-dihydroquinoline-3-carboxylic acid収率 95.3%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

To 400 mg of the mixed solution (1:1) of 4N hydrochloric acid and acetic acid was added 35 mg of ethyl 1-(4-amino-5-fluoropyridin-2-yl)-8-chloro-6,7-difluoro-4-oxo-1,4-dihydroquinoline-3-carboxylate, and the mixture was heated under reflux with stirring for 3 hours and allowed to cool. The precipitate was collected by filtration, and washed with distilled water, ethanol and diisopropylether successively to obtain 31 mg of the title compound as a pale yellow powder.

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux
  3. temperatureto cool
  4. filtrationThe precipitate was collected by filtration
  5. washwashed with distilled water, ethanol and diisopropylether successively

出典と根拠

ORDレコード
ord-72a48e2ab03940d8ac50d2dcfacc2eef
出典データセット
uspto-grants-1999_12
特許番号
US05998436

反応ノート

読み込み中…