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Hydrochloric Acid → 5-Amino-1-cyclopropyl-6,8-difluoro-7-(3-methyl-1-piperazinyl)-1,4-dihydro-4-oxoquinoline-3-carboxylic acid hydrochloride

HRID 2291288
ノート
印刷プレビュー

反応式

HRID 2291288 の反応式
[CH:1]1([N:4]2[C:13]3[C:8](=[C:9]([NH:23]C(OCC)=O)[C:10]([F:22])=[C:11]([N:15]4[CH2:20][CH2:19][NH:18][CH:17]([CH3:21])[CH2:16]4)[C:12]=3[F:14])[C:7](=[O:29])[C:6]([C:30]([O:32]CC)=[O:31])=[CH:5]2)[CH2:3][CH2:2]1.[OH-].[Na+].[ClH:37]>C(O)C>[ClH:37].[NH2:23][C:9]1[C:10]([F:22])=[C:11]([N:15]2[CH2:20][CH2:19][NH:18][CH:17]([CH3:21])[CH2:16]2)[C:12]([F:14])=[C:13]2[C:8]=1[C:7](=[O:29])[C:6]([C:30]([OH:32])=[O:31])=[CH:5][N:4]2[CH:1]1[CH2:3][CH2:2]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 21279709Ethyl 1-cyclopropyl-5-ethoxycarbonylamino-6,8-difluoro-7-(3-methyl-1-piperazinyl)-1,4-dihydro-4-oxoquinoline-3-carboxylate

生成物 1

HCID 679476925-Amino-1-cyclopropyl-6,8-difluoro-7-(3-methyl-1-piperazinyl)-1,4-dihydro-4-oxoquinoline-3-carboxylic acid hydrochloride

試薬・触媒・溶媒 1

HCID 702
Ethanol
溶媒

実験手順

A mixture of ethyl 1-cyclopropyl-5-ethoxycarbonylamino-6,8-difluoro-7-(3-methyl-1-piperazinyl)-1,4-dihydro-4-oxoquinoline-3-carboxylate, 20% aqueous sodium hydroxide, and ethanol was refluxed for 12 hours. The reaction mixture was treated with activated carbon and adjusted at pH 1-2 with 10% hydrochloric acid. After cooling, the resulting crystals were collected by filtration and recrystallization from water-ethanol to give 5-amino-1-cyclopropyl-6,8-difluoro-7-(3-methyl-1-piperazinyl)-1,4-dihydro-4-oxoquinoline-3-carboxylic acid hydrochloride, m.p. >300° C.

後処理

  1. temperaturewas refluxed for 12 hours
  2. additionThe reaction mixture was treated with activated carbon
  3. temperatureAfter cooling
  4. filtrationthe resulting crystals were collected by filtration and recrystallization from water-ethanol

出典と根拠

ORDレコード
ord-09334dd78d5f4611a10516869370b268
出典データセット
uspto-grants-1989_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04795751

反応ノート

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