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

HRID 1031581노트

반응식

HRID 1031581 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.[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 물질

4

반응물 2

HCID 5360545SodiumHCID 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 hydroxyde 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-c8bf65bb93124232b015be934b17abd5
출처 데이터셋
uspto-grants-1990_09
특허 번호
US04954507

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