Sodium Acetate → 1-Cyclopropyl-6,8-difluoro-1,4-dihydro-7-(2,6-dimethyl-4-pyridinyl)-4-oxo-3-quinolinecarboxyic acid

HRID 1461386노트

반응식

HRID 1461386 반응식
[CH:1]1([N:4]2[C:13]3[C:8](=[CH:9][C:10]([F:23])=[C:11]([C:15]4[CH:20]=[C:19]([CH3:21])[N:18]=[C:17]([CH3:22])[CH:16]=4)[C:12]=3[F:14])[C:7](=[O:24])[C:6]([C:25]([O:27]CC)=[O:26])=[CH:5]2)[CH2:3][CH2:2]1.C([O-])(=O)C.[Na+]>Cl>[CH:1]1([N:4]2[C:13]3[C:8](=[CH:9][C:10]([F:23])=[C:11]([C:15]4[CH:20]=[C:19]([CH3:21])[N:18]=[C:17]([CH3:22])[CH:16]=4)[C:12]=3[F:14])[C:7](=[O:24])[C:6]([C:25]([OH:27])=[O:26])=[CH:5]2)[CH2:3][CH2:2]1

참가 물질

4

반응물 2

HCID 517045Sodium AcetateHCID 9978175HCID 9978175, 화합물

생성물 1

HCID 1300781-Cyclopropyl-6,8-difluoro-1,4-dihydro-7-(2,6-dimethyl-4-pyridinyl)-4-oxo-3-quinolinecarboxyic acid수율 75.3%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

A suspension of 1.0 g ethyl 1-cyclopropyl-6,8-difluoro-7-(2,6-dimethyl-4-pyridinyl)-1,4-dihydro-4-oxo-3-quinolinecarboxylate in 20 ml 1M hydrochloric acid was heated at reflux for 2 hours. The reaction mixture was cooled, poured into saturated sodium acetate and extracted with ethyl acetate. The extract was dried (sodium sulfate) and concentrated, and the residue (0.84 g) was recrystallized from absolute ethanol to give 0.70 g 1-cyclopropyl-6,8-difluoro-7-(2,6-dimethyl-4-pyridinyl)-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid, colorless needles, m.p. 246°-248.5° C.

후처리

  1. temperaturewas heated
  2. temperatureat reflux for 2 hours
  3. temperatureThe reaction mixture was cooled
  4. extractionextracted with ethyl acetate
  5. dry with materialThe extract was dried (sodium sulfate)
  6. concentrationconcentrated
  7. customthe residue (0.84 g) was recrystallized from absolute ethanol

출처 및 근거

ORD 기록
ord-4d5f22cb6b764c98926835330a5d690a
출처 데이터셋
uspto-grants-1991_12
특허 번호
US05075319

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