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

HRID 34576
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반응식

HRID 34576 반응식
[CH:1]1([N:4]2[C:13]3[C:8](=[CH:9][C:10]([F:16])=[C:11]([CH3:15])[C:12]=3[F:14])[C:7](=[O:17])[C:6]([C:18]([O:20]CC)=[O:19])=[CH:5]2)[CH2:3][CH2:2]1.C(O)(=O)C.S(=O)(=O)(O)O>O>[CH:1]1([N:4]2[C:13]3[C:8](=[CH:9][C:10]([F:16])=[C:11]([CH3:15])[C:12]=3[F:14])[C:7](=[O:17])[C:6]([C:18]([OH:20])=[O:19])=[CH:5]2)[CH2:2][CH2:3]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 1118Sulfuric AcidHCID 13657408Ethyl 1-cyclopropyl-6,8-difluoro-7-methyl-1,4-dihydro-4-oxo-3-quinolinecarboxylate

생성물 1

HCID 136574231-Cyclopropyl-6,8-difluoro-7-methyl-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid수율 95%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 30 g of ethyl 1-cyclopropyl-6,8-difluoro-7-methyl-1,4-dihydro-4-oxo-3-quinolinecarboxylate, 210 ml of glacial acetic acid, 160 ml of water and 23.5 ml of concentrated sulphuric acid is heated under reflux for 2 hours. The hot suspension is then poured onto ice and the precipitate is filtered off with suction, rinsed thoroughly with water and dried in vacuo at 100° C. 25.9 g of pure 1-cyclopropyl-6,8-difluoro-7-methyl-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid of melting point 227°-229° C. are obtained in this manner.

후처리

  1. temperatureis heated
  2. temperatureunder reflux for 2 hours
  3. additionThe hot suspension is then poured onto ice
  4. filtrationthe precipitate is filtered off with suction
  5. washrinsed thoroughly with water
  6. customdried in vacuo at 100° C

출처 및 근거

ORD 기록
ord-278dd9c5777f4bd4926a60756f704be2
출처 데이터셋
uspto-grants-1988_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04762844

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