Acetic Acid → HCID 4914114、化合物

HRID 2291286ノート

反応式

HRID 2291286 の反応式
C([NH:8][C:9]1[C:18]([F:19])=[C:17]([N:20]2[CH2:25][CH2:24][N:23]([CH3:26])[CH2:22][CH2:21]2)[C:16]([F:27])=[C:15]2[C:10]=1[C:11](=[O:34])[C:12]([C:31]([OH:33])=[O:32])=[CH:13][N:14]2[CH:28]1[CH2:30][CH2:29]1)C1C=CC=CC=1.C(O)(=O)C>[C].[Pd].C(O)C>[NH2:8][C:9]1[C:18]([F:19])=[C:17]([N:20]2[CH2:21][CH2:22][N:23]([CH3:26])[CH2:24][CH2:25]2)[C:16]([F:27])=[C:15]2[C:10]=1[C:11](=[O:34])[C:12]([C:31]([OH:33])=[O:32])=[CH:13][N:14]2[CH:28]1[CH2:30][CH2:29]1

参加物

5

反応物 2

HCID 176Acetic AcidHCID 146641725-Benzylamino-1-cyclopropyl-6,8-difluoro-7-(4-methyl-1-piperazinyl)-1,4-dihydro-4-oxoquinoline-3-carboxylic acid

生成物 1

HCID 4914114HCID 4914114、化合物収率 90.2%

試薬・触媒・溶媒 2

HCID 178418390HCID 178418390、化合物触媒HCID 702Ethanol溶媒

実験手順

A mixture of 5-benzylamino-1-cyclopropyl-6,8-difluoro-7-(4-methyl-1-piperazinyl)-1,4-dihydro-4-oxoquinoline-3-carboxylic acid (700 mg), 5% palladium-carbon (0.2 g), acetic acid (10 ml), and ethanol (15 ml) was stirred at room temperature for 30 minutes under a hydrogen stream. The catalyst was filtered off and the filtrate was evaporated under reduced pressure. After addition of water to the residue, the mixture was adjusted to pH 8 with aqueous ammonia. The resulting crystals were filtered to give 5-amino-1-cyclopropyl-6,8-difluoro-7-(4-methyl-1-piperazinyl)-1,4-dihydro-4-oxoquinoline-3-carboxylic acid (510 mg), m.p. 254°-255° C.

後処理

  1. filtrationThe catalyst was filtered off
  2. customthe filtrate was evaporated under reduced pressure
  3. additionAfter addition of water to the residue
  4. filtrationThe resulting crystals were filtered

出典と根拠

ORDレコード
ord-0b78857c83e54f38971dac3414b8c17f
出典データセット
uspto-grants-1989_01
特許番号
US04795751

反応ノート

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