Sodium Acetate → 1-Cyclopropyl-6,8-difluoro-1,4-dihydro-7-(2,6-dimethyl-4-pyridinyl)-4-oxo-3-quinolinecarboxyic acid

HRID 1681195ノート

反応式

HRID 1681195 の反応式
[CH:1]1([N:4]2[C:13]3[C:8](=[CH:9][C:10]([F:23])=[C:11]([C:15]4[CH:20]=[C:19]([CH3:21])[N:18]=[C:17]([CH3:22])[CH:16]=4)[C:12]=3[F:14])[C:7](=[O:24])[C:6]([C:25]([O:27]CC)=[O:26])=[CH:5]2)[CH2:3][CH2:2]1.C([O-])(=O)C.[Na+]>Cl>[CH:1]1([N:4]2[C:13]3[C:8](=[CH:9][C:10]([F:23])=[C:11]([C:15]4[CH:20]=[C:19]([CH3:21])[N:18]=[C:17]([CH3:22])[CH:16]=4)[C:12]=3[F:14])[C:7](=[O:24])[C:6]([C:25]([OH:27])=[O:26])=[CH:5]2)[CH2:3][CH2:2]1

参加物

4

反応物 2

HCID 517045Sodium AcetateHCID 9978175HCID 9978175、化合物

生成物 1

HCID 1300781-Cyclopropyl-6,8-difluoro-1,4-dihydro-7-(2,6-dimethyl-4-pyridinyl)-4-oxo-3-quinolinecarboxyic acid収率 75.3%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

A suspension of 1.0 g ethyl 1-cyclopropyl-6,8-difluoro-7-(2,6-dimethyl-4-pyridinyl)-1,4-dihydro-4-oxo-3-quinolinecarboxylate in 20 ml 1M hydrochloric acid was heated at reflux for 2 hours. The reaction mixture was cooled, poured into saturated sodium acetate and extracted with ethyl acetate. The extract was dried (sodium sulfate) and concentrated, and the residue (0.84 g) was recrystallized from absolute ethanol to give 0.70 g 1-cyclopropyl-6,8-difluoro-7-(2,6-dimethyl-4-pyridinyl)-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid, colorless needles, m.p. 246°-248.5° C.

後処理

  1. temperaturewas heated
  2. temperatureat reflux for 2 hours
  3. temperatureThe reaction mixture was cooled
  4. extractionextracted with ethyl acetate
  5. dry with materialThe extract was dried (sodium sulfate)
  6. concentrationconcentrated
  7. customthe residue (0.84 g) was recrystallized from absolute ethanol

出典と根拠

ORDレコード
ord-ade365c33b2147ec8249800c9d6fa12c
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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