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7-(4-Benzyl-1-piperazinyl)-1-cyclopropyl-6-fluoro-8-methyl-1,4-dihydro-4-oxoquinoline-3-carboxylic acid → 7-(1-Piperazinyl)-1-cyclopropyl-6-fluoro-8-methyl-1,4-dihydro-4-oxoquinoline-3-carboxylic acid

HRID 1638688
ノート
印刷プレビュー

反応式

HRID 1638688 の反応式
C([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[C:23]([CH3:24])=[C:22]3[C:17]([C:18](=[O:31])[C:19]([C:28]([OH:30])=[O:29])=[CH:20][N:21]3[CH:25]3[CH2:27][CH2:26]3)=[CH:16][C:15]=2[F:32])[CH2:10][CH2:9]1)C1C=CC=CC=1>[Pd].C(O)(=O)C>[N:11]1([C:14]2[C:23]([CH3:24])=[C:22]3[C:17]([C:18](=[O:31])[C:19]([C:28]([OH:30])=[O:29])=[CH:20][N:21]3[CH:25]3[CH2:26][CH2:27]3)=[CH:16][C:15]=2[F:32])[CH2:12][CH2:13][NH:8][CH2:9][CH2:10]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 156224987-(4-Benzyl-1-piperazinyl)-1-cyclopropyl-6-fluoro-8-methyl-1,4-dihydro-4-oxoquinoline-3-carboxylic acid

生成物 1

HCID 140525807-(1-Piperazinyl)-1-cyclopropyl-6-fluoro-8-methyl-1,4-dihydro-4-oxoquinoline-3-carboxylic acid収率 67.6%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 176Acetic Acid溶媒

実験手順

To 7-(4-benzyl-1-piperazinyl)-1-cyclopropyl-6-fluoro-8-methyl-1,4 -dihydro-4-oxoquinoline-3-carboxylic acid (84 mg) are added acetic acid (3 ml) and 10% Pd-C (10 mg), and the mixture is subjected to catalytic reduction at 70° C. for one hour. After the catalytic reduction, the reaction mixture is cooled and the catalyst is filtered off. The filtrate is concentrated, and to the residue is added aqueous sodium hydrogen carbonate, and the resulting precipitates are separated by filtration to give 7-(1-piperazinyl)-1-cyclopropyl-6-fluoro-8-methyl-1,4-dihydro-4-oxoquinoline-3-carboxylic acid (45 mg), as white crystals, m.p. 291°-295° C. (decomp.).

後処理

  1. temperatureAfter the catalytic reduction, the reaction mixture is cooled
  2. filtrationthe catalyst is filtered off
  3. concentrationThe filtrate is concentrated
  4. additionto the residue is added aqueous sodium hydrogen carbonate
  5. customthe resulting precipitates
  6. customare separated by filtration

出典と根拠

ORDレコード
ord-04fc42fc1d1b40b7ba932476ba51b922
出典データセット
uspto-grants-1989_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04880806

反応ノート

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