Methane → Win 57273

HRID 1681187ノート

反応式

HRID 1681187 の反応式
[CH:1]1([N:4]2[C:13]3[C:8](=[CH:9][C:10]([F:22])=[C:11]([C:14]4[CH:19]=[C:18]([CH3:20])[N:17]=[C:16]([CH3:21])[CH:15]=4)[CH:12]=3)[C:7](=[O:23])[C:6]([C:24]([O:26]CC)=[O:25])=[CH:5]2)[CH2:3][CH2:2]1.C>O>[CH:1]1([N:4]2[C:13]3[C:8](=[CH:9][C:10]([F:22])=[C:11]([C:14]4[CH:15]=[C:16]([CH3:21])[N:17]=[C:18]([CH3:20])[CH:19]=4)[CH:12]=3)[C:7](=[O:23])[C:6]([C:24]([OH:26])=[O:25])=[CH:5]2)[CH2:3][CH2:2]1

参加物

4

反応物 2

HCID 297MethaneHCID 9999813Ethyl 1-cyclopropyl-7-(2,6-dimethyl-4-pyridinyl)6-fluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylate

生成物 1

HCID 121960Win 57273収率 73.1%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A suspension of 12.4 g ethyl 1-cyclopropyl-7-(2,6-dimethyl-4-pyridinyl)-6-fluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylate in 320 ml water containing 3.5 g sodium hydroxide was heated at reflux for 2.5 hours. The reaction mixture was then decolorized with charcoal, filtered and brought to pH 5-5.5 with acetic acid. The solid that precipitated was collected, dried in vacuo and recrystallized from dimethylformamide to give 8.4 g 1-cyclopropyl-7-(2,6-dimethyl-4-pyridinyl)-6-fluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid, m.p. 300°-302° C.(decompn.).

後処理

  1. temperaturewas heated
  2. temperatureat reflux for 2.5 hours
  3. filtrationfiltered
  4. customThe solid that precipitated
  5. customwas collected
  6. customdried in vacuo
  7. customrecrystallized from dimethylformamide

出典と根拠

ORDレコード
ord-3b983bd148ee4da4896e902f0e77642a
出典データセット
uspto-grants-1992_12
特許番号
US05169853

反応ノート

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