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Hydrochloric Acid → 5-Amino-1-cyclopropyl-6,7-difluoro-8-methyl-4-oxo-1,4-dihydroquinoline-3-carboxylic acid

HRID 1078269
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반응식

HRID 1078269 반응식
[NH2:1][C:2]1[C:11]([F:12])=[C:10]([F:13])[C:9]([CH3:14])=[C:8]2[C:3]=1[C:4](=[O:23])[C:5]([C:18]([O:20]CC)=[O:19])=[CH:6][N:7]2[CH:15]1[CH2:17][CH2:16]1.Cl>C(O)(=O)C>[NH2:1][C:2]1[C:11]([F:12])=[C:10]([F:13])[C:9]([CH3:14])=[C:8]2[C:3]=1[C:4](=[O:23])[C:5]([C:18]([OH:20])=[O:19])=[CH:6][N:7]2[CH:15]1[CH2:17][CH2:16]1
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참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 10519846Ethyl 5-amino-1-cyclopropyl-6,7-difluoro-8-methyl-4-oxo-1,4-dihydroquinoline-3-carboxylate

생성물 1

HCID 108513065-Amino-1-cyclopropyl-6,7-difluoro-8-methyl-4-oxo-1,4-dihydroquinoline-3-carboxylic acid수율 87.3%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

A mixture of 14.8 g of ethyl 5-amino-1-cyclopropyl-6,7-difluoro-1,4-dihydro-8-methyl-4-oxoquinoline-3-carboxylate, 37.2 ml of hydrochloric acid and 150 ml of 90% acetic acid was heated at reflux for 2 hours. After cooling, the deposited crystals were collected by filtration and washed with water to give 11.8 g of the desired compound as yellow crystals. The crystals were subsequently recrystallized from N,N-dimethylformamide to give yellow crystals, m.p. 290.5° C. (decomp.).

후처리

  1. temperaturewas heated
  2. temperatureat reflux for 2 hours
  3. temperatureAfter cooling
  4. filtrationthe deposited crystals were collected by filtration
  5. washwashed with water

출처 및 근거

ORD 기록
ord-bf7126cbe977486cb976473a13ab3c01
출처 데이터셋
uspto-grants-1996_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05547962

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