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Sodium Hydroxide → 1-(1,1-Dimethylethyl)-1,4-dihydro-6,7-difluoro-4-oxo-3-quinolinecarboxylic acid

HRID 1089223
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반응식

HRID 1089223 반응식
C([O:3][C:4]([C:6]1[C:15](=[O:16])[C:14]2[C:9](=[CH:10][C:11]([F:18])=[C:12]([F:17])[CH:13]=2)[N:8]([C:19]([CH3:22])([CH3:21])[CH3:20])[CH:7]=1)=[O:5])C.[OH-].[Na+]>C(O)C>[F:17][C:12]1[CH:13]=[C:14]2[C:9](=[CH:10][C:11]=1[F:18])[N:8]([C:19]([CH3:21])([CH3:22])[CH3:20])[CH:7]=[C:6]([C:4]([OH:5])=[O:3])[C:15]2=[O:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 14612522HCID 14612522, 화합물

생성물 1

HCID 148395931-(1,1-Dimethylethyl)-1,4-dihydro-6,7-difluoro-4-oxo-3-quinolinecarboxylic acid

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 6.08 g (19.7 mmoles) of 6,7-difluoro-1-(1,1-dimethylethyl)-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid ethyl ester and 19.7 mmoles of 2N aqueous sodium hydroxide in 80 mL of ethanol was stirred overnight. The resulting mixture was concentrated in vacuo, taken up with 200 mL of water and extracted with dichloromethane. About 8 mL of 2N HCl was added to the aqueous layer to adjust the pH to 3. The precipitate was collected by filtration, washed with H2O and dried to give 4.47 g, of titled compound. MP >260° C.

후처리

  1. concentrationThe resulting mixture was concentrated in vacuo
  2. extractionextracted with dichloromethane
  3. additionAbout 8 mL of 2N HCl was added to the aqueous layer
  4. filtrationThe precipitate was collected by filtration
  5. washwashed with H2O
  6. customdried
  7. customto give 4.47 g

출처 및 근거

ORD 기록
ord-db219fd19ba64714b473a95e754fff39
출처 데이터셋
uspto-grants-1990_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04965273

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