Formaldehyde → 7-(3,4-Dimethyl-1-piperazinyl)-1-ethyl-6,8-difluoro-1,4-dihydro-4-oxoquinoline-3-carboxlic acid

HRID 370715ノート

反応式

HRID 370715 の反応式
[CH2:1]([N:3]1[C:12]2[C:7](=[CH:8][C:9]([F:21])=[C:10]([N:14]3[CH2:19][CH2:18][NH:17][CH:16]([CH3:20])[CH2:15]3)[C:11]=2[F:13])[C:6](=[O:22])[C:5]([C:23]([OH:25])=[O:24])=[CH:4]1)[CH3:2].[CH2:26]=O>C(O)=O>[CH3:20][CH:16]1[N:17]([CH3:26])[CH2:18][CH2:19][N:14]([C:10]2[C:11]([F:13])=[C:12]3[C:7]([C:6](=[O:22])[C:5]([C:23]([OH:25])=[O:24])=[CH:4][N:3]3[CH2:1][CH3:2])=[CH:8][C:9]=2[F:21])[CH2:15]1

参加物

4

反応物 2

HCID 712FormaldehydeHCID 3948Lomefloxacin

生成物 1

HCID 134776637-(3,4-Dimethyl-1-piperazinyl)-1-ethyl-6,8-difluoro-1,4-dihydro-4-oxoquinoline-3-carboxlic acid

試薬・触媒・溶媒 1

HCID 284Formic Acid溶媒

実験手順

A mixture of 1.40 g of 1-ethyl-6,8-difluoro-1,4-dihydro-7-(3-methyl-1-piperazinyl)-4-oxoquinoline-3-carboxylic acid, 2.8 ml of 90% formic acid and 2.2 ml of 37% formalin was heated for 4 hours under reflux. The reaction mixture was evaporated and the residue was dissolved in water. The solution was neutralized with aqueous sodium bicarbonate. The precipitate was filtered and recrystallized from ethanol to give 0.32 g of the title compound as colorless needles, M.p. 211.5°-212° C.

後処理

  1. temperaturewas heated for 4 hours
  2. temperatureunder reflux
  3. customThe reaction mixture was evaporated
  4. dissolutionthe residue was dissolved in water
  5. filtrationThe precipitate was filtered
  6. customrecrystallized from ethanol

出典と根拠

ORDレコード
ord-841b7245c77b43c88fd1851b8beb19af
出典データセット
uspto-grants-1985_07
特許番号
US04528287

反応ノート

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