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Hydrochloric Acid → 1-Ethyl-6-fluoro-7-hydroxy-1,4-dihydro-4-oxo-quinoline-3-carboxylic acid

HRID 963394
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HRID 963394 반응식
[CH2:1]([N:3]1[C:12]2[C:7](=[CH:8][C:9]([F:14])=[C:10](F)[CH:11]=2)[C:6](=[O:15])[C:5]([C:16]([O:18]CC)=[O:17])=[CH:4]1)[CH3:2].Cl.[OH-:22].[Na+]>>[CH2:1]([N:3]1[C:12]2[C:7](=[CH:8][C:9]([F:14])=[C:10]([OH:22])[CH:11]=2)[C:6](=[O:15])[C:5]([C:16]([OH:18])=[O:17])=[CH:4]1)[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 854165Ethyl 1-ethyl-6,7-difluoro-4-oxo-1,4-dihydroquinoline-3-carboxylate

생성물 1

HCID 166386641-Ethyl-6-fluoro-7-hydroxy-1,4-dihydro-4-oxo-quinoline-3-carboxylic acid수율 91%

실험 절차

A suspension of 1.2 g of ethyl 1-ethyl-6,7-difluoro-1,4-dihydro-4-oxo-quinoline-3-carboxylate (European Offenlegungsschrift No. 230053, C.A. 108:112498) in 25 ml of 2N aqueous sodium hydroxide solution is heated at reflux for 4 hrs. After cooling to room temperature the reaction mixture is adjusted to pH 3 to 4 with 37% aqueous hydrochloric acid and the precipitate is filtered off under suction, washed with 200 ml of water and 200 ml of diethyl ether and dried. 980 mg (91%) of 1-ethyl-6-fluoro-7-hydroxy-1,4-dihydro-4-oxo-quinoline-3-carboxylic acid are isolated as a colourless solid. M.p.>250°.

후처리

  1. temperatureis heated
  2. temperatureat reflux for 4 hrs
  3. filtrationthe precipitate is filtered off under suction
  4. washwashed with 200 ml of water and 200 ml of diethyl ether
  5. customdried

출처 및 근거

ORD 기록
ord-ab4a868cead744468bd80a40271c8e45
출처 데이터셋
uspto-grants-1998_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05763450

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