Hydrochloric Acid → Moxifloxacin difluoro methoxy ethyl ester

HRID 358879노트

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HRID 358879 반응식
[H-].[Na+].[CH:3]1([NH:6][CH:7]=[C:8]([C:14](=[O:26])[C:15]2[CH:20]=[C:19]([F:21])[C:18]([F:22])=[C:17]([O:23][CH3:24])[C:16]=2F)[C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH2:5][CH2:4]1.Cl>O1CCCC1>[CH:3]1([N:6]2[C:16]3[C:15](=[CH:20][C:19]([F:21])=[C:18]([F:22])[C:17]=3[O:23][CH3:24])[C:14](=[O:26])[C:8]([C:9]([O:11][CH2:12][CH3:13])=[O:10])=[CH:7]2)[CH2:5][CH2:4]1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 24758Sodium hydrideHCID 178471878HCID 178471878, 화합물

생성물 1

HCID 10758239Moxifloxacin difluoro methoxy ethyl ester수율 73.4%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

150 mg (0.0035 mole) of sodium hydride (as a 60% w/w dispersion in mineral oil) were added to a solution of 1.20 g (0.0035 mole) of ethyl 3-cyclopropylamino-2-(3-methoxy-2,4,5-trifluorobenzoyl)acrylate (XXXI) [prepared as described in Step (E11) above] in 30 ml of anhydrous tetrahydrofuran, and the mixture was stirred at room temperature for 30 minutes. At the end of this time, the reaction mixture was acidified by adding 1N aqueous hydrochloric acid, and the mixture was extracted with ethyl acetate. The extract was washed with water and dried, and the solvent was removed by evaporation under reduced pressure to afford 0.83 g of ethyl 1-cyclopropyl-6,7-difluoro-8-methoxy-1,4-dihydro-4-oxoquinoline-3-carboxylate (XXXII) as colorless needles, melting at 180°-182° C.

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe extract was washed with water
  3. customdried
  4. customthe solvent was removed by evaporation under reduced pressure

출처 및 근거

ORD 기록
ord-8437bba81e8e4a898e83cb65d92e0d7a
출처 데이터셋
uspto-grants-1991_03
특허 번호
US04997943

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