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Acetic Acid → 8-Bromo-1-cyclopropyl-6,7-difluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid

HRID 1761654
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반응식

HRID 1761654 반응식
[Br:1][C:2]1[C:3]([F:22])=[C:4]([F:21])[CH:5]=[C:6]2[C:11]=1[N:10]([CH:12]1[CH2:14][CH2:13]1)[CH:9]=[C:8]([C:15]([O:17]CC)=[O:16])[C:7]2=[O:20].C(O)(=O)C.S(=O)(=O)(O)O>O>[Br:1][C:2]1[C:3]([F:22])=[C:4]([F:21])[CH:5]=[C:6]2[C:11]=1[N:10]([CH:12]1[CH2:14][CH2:13]1)[CH:9]=[C:8]([C:15]([OH:17])=[O:16])[C:7]2=[O:20]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 1118Sulfuric AcidHCID 11046932Ethyl 8-bromo-1-cyclopropyl-6,7-difluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylate

생성물 1

HCID 137488068-Bromo-1-cyclopropyl-6,7-difluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid수율 88.7%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of ethyl 8-bromo-1-cyclopropyl-6,7-difluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylate (1.0 g), acetic acid (4 ml), water (3 ml) and concentrated sulfuric acid (0.5 ml) was heated on an oil bath (90°-100° C.) for an hour under stirring, then for an hour at room temperature and poured into ice water (20 ml). The resulting precipitate was collected by filtration and washed with water to give the title compound (0.82 g), mp 224°-225.5° C.

후처리

  1. temperaturewas heated on an oil bath (90°-100° C.) for an hour
  2. waitfor an hour at room temperature
  3. filtrationThe resulting precipitate was collected by filtration
  4. washwashed with water

출처 및 근거

ORD 기록
ord-77311101f02b4f1b8c78a2f83b976ca4
출처 데이터셋
uspto-grants-1989_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04826982

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