Moxifloxacin difluoro methoxy ethyl ester → 1-Cyclopropyl-6,7-difluoro-8-hydroxy-4-oxo-1,4-dihydroquinoline-3-carboxylic acid

HRID 2356380ノート

反応式

HRID 2356380 の反応式
[CH:1]1([N:4]2[C:13]3[C:8](=[CH:9][C:10]([F:17])=[C:11]([F:16])[C:12]=3[O:14]C)[C:7](=[O:18])[C:6]([C:19]([O:21]CC)=[O:20])=[CH:5]2)[CH2:3][CH2:2]1>Br.C(O)(=O)C>[CH:1]1([N:4]2[C:13]3[C:8](=[CH:9][C:10]([F:17])=[C:11]([F:16])[C:12]=3[OH:14])[C:7](=[O:18])[C:6]([C:19]([OH:21])=[O:20])=[CH:5]2)[CH2:2][CH2:3]1

参加物

4

反応物 1

HCID 10758239Moxifloxacin difluoro methoxy ethyl ester

生成物 1

HCID 116807371-Cyclopropyl-6,7-difluoro-8-hydroxy-4-oxo-1,4-dihydroquinoline-3-carboxylic acid収率 89.8%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 260Hydrogen Bromide溶媒

実験手順

The preparation comprises dissolving Ethyl 1-cyclopropyl-6,7-difluoro-8-methoxy-1,4-dihydro-4-oxoquinoline-3-carboxylate (10.0 g, 30.9 mmol) in 40% HBr aqueous solution (20 mL) and acetic acid (20 mL) to react at 100° C., charging reaction mixture into ice water (500 mL) under fast stirring after the reaction finishes, going on with the stirring for 0.5 h, filtering, and drying obtained filter cake to give 1-cyclopropyl-6,7-difluoro-8-hydroxy-1,4-dihydro-oxoquinoline-3-carboxylic acid (7.8 g, 89.6%).

後処理

  1. customto react at 100° C.
  2. customstirring for 0.5 h
  3. filtrationfiltering
  4. customdrying
  5. customobtained
  6. filtrationfilter cake

出典と根拠

ORDレコード
ord-41eeed3c861a4e169441e5ed565efd7a
出典データセット
uspto-grants-2010_07
特許番号
US07759362B2

反応ノート

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