5-Benzylamino-1-cyclopropyl-6,7-difluoro-1,4-dihydro-4-oxoquinoline-3-carboxylic acid → 7-(4-Acetyl-3-methyl-1-piperazinyl)-5-benzylamino-1-cyclopropyl-6-fluoro-1,4-dihydro-4-oxoquinoline-3-carboxylic acid

HRID 373527ノート

反応式

HRID 373527 の反応式
[CH2:1]([NH:8][C:9]1[C:18]([F:19])=[C:17](F)[CH:16]=[C:15]2[C:10]=1[C:11](=[O:27])[C:12]([C:24]([OH:26])=[O:25])=[CH:13][N:14]2[CH:21]1[CH2:23][CH2:22]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:28]([N:31]1[CH2:36][CH2:35][NH:34][CH2:33][CH:32]1[CH3:37])(=[O:30])[CH3:29]>N1C=CC=CC=1>[C:28]([N:31]1[CH2:36][CH2:35][N:34]([C:17]2[CH:16]=[C:15]3[C:10]([C:11](=[O:27])[C:12]([C:24]([OH:26])=[O:25])=[CH:13][N:14]3[CH:21]3[CH2:23][CH2:22]3)=[C:9]([NH:8][CH2:1][C:2]3[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=3)[C:18]=2[F:19])[CH2:33][CH:32]1[CH3:37])(=[O:30])[CH3:29]

参加物

4

実験手順

A mixture of 5-benzylamino-1-cyclopropyl-6,7-difluoro-1,4-dihydro-4-oxoquinoline-3-carboxylic acid, 1-acetyl-2-methylpiperazine and pyridine was heated under reflux. The reaction mixture was concentrated under reduced pressure, and water was added to the residue. The mixture was extracted with chloroform. The extract was dried and chloroform was evaporated. Ethanol was added to the residue, and the crystals were collected by filtration to give 7-(4-acetyl-3-methyl-1-piperazinyl)-5-benzylamino-1-cyclopropyl-6-fluoro-1,4-dihydro-4-oxoquinoline-3-carboxylic acid. It was recrystallized from ethanol/diisopropyl ether. m.p. 235°-236° C.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux
  3. concentrationThe reaction mixture was concentrated under reduced pressure, and water
  4. additionwas added to the residue
  5. extractionThe mixture was extracted with chloroform
  6. customThe extract was dried
  7. customchloroform was evaporated
  8. additionEthanol was added to the residue
  9. filtrationthe crystals were collected by filtration

出典と根拠

ORDレコード
ord-6f70d3e97d024bb8b1fb7792cd699205
出典データセット
uspto-grants-1992_11
特許番号
US05164392

反応ノート

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