Methane → Win 57273

HRID 1461379ノート

反応式

HRID 1461379 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-f6c01132972c4455919dd75579cd5eb1
出典データセット
uspto-grants-1991_12
特許番号
US05075319

反応ノート

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