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

HRID 486274

反応式

HRID 486274 の反応式
[N:1]1([C:7]2[CH:16]=[C:15]3[C:10]([C:11](=[O:23])[C:12]([C:20]([OH:22])=[O:21])=[CH:13][N:14]3[CH:17]3[CH2:19][CH2:18]3)=[C:9]([CH3:24])[C:8]=2[F:25])[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.[C:26](OC(=O)C)(=[O:28])[CH3:27].Cl>[OH-].[Na+]>[C:26]([N:4]1[CH2:5][CH2:6][N:1]([C:7]2[CH:16]=[C:15]3[C:10]([C:11](=[O:23])[C:12]([C:20]([OH:22])=[O:21])=[CH:13][N:14]3[CH:17]3[CH2:18][CH2:19]3)=[C:9]([CH3:24])[C:8]=2[F:25])[CH2:2][CH2:3]1)(=[O:28])[CH3:27]

参加物

5

実験手順

To a solution of 7-(1-piperazinyl)-1-cyclopropyl-6-fluoro-5-methyl-1,4-dihydro-4-oxoquinoline-3-carboxylic acid (40 mg) in 5% sodium hydroxide (2 ml) is added acetic anhydride (0.1 ml) at room temperature. After the mixture is made acidic with dilute hydrochloric acid, the resultant product is extracted with dichloromethane and the extract is dried over magnesium sulfate. After concentrating, the obtained residue is recrystallized from ethanol to give 7-(4-acetyl-1-piperazinyl)-1 -cyclopropyl-6-fluoro-5-methyl-1,4-dihydro-4-oxoquinoline-3-carboxylic acid (29 mg), as white powder, m.p. 261°-263° C.

後処理

  1. extractionthe resultant product is extracted with dichloromethane
  2. dry with materialthe extract is dried over magnesium sulfate
  3. concentrationAfter concentrating
  4. customthe obtained residue is recrystallized from ethanol

出典と根拠

ORDレコード
ord-52ebd7a90df44c81811199bf14d2f00d
出典データセット
uspto-grants-1994_03
特許番号
US05290934

関連ノート

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