Hydrochloric Acid → 1-Cyclopropyl-6,7-difluoro-1,4-dihydro-8-methoxy-4-oxo-3-quinolinecarboxylic acid

HRID 358880

반응식

HRID 358880 반응식
[OH-].[Na+].[CH:3]1([N:6]2[C:15]3[C:10](=[CH:11][C:12]([F:19])=[C:13]([F:18])[C:14]=3[O:16][CH3:17])[C:9](=[O:20])[C:8]([C:21]([O:23]CC)=[O:22])=[CH:7]2)[CH2:5][CH2:4]1.Cl>CO>[CH:3]1([N:6]2[C:15]3[C:10](=[CH:11][C:12]([F:19])=[C:13]([F:18])[C:14]=3[O:16][CH3:17])[C:9](=[O:20])[C:8]([C:21]([OH:23])=[O:22])=[CH:7]2)[CH2:4][CH2:5]1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 10758239Moxifloxacin difluoro methoxy ethyl ester

생성물 1

HCID 70194651-Cyclopropyl-6,7-difluoro-1,4-dihydro-8-methoxy-4-oxo-3-quinolinecarboxylic acid수율 76.8%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

10 ml of a 4% w/v aqueous solution of sodium hydroxide were added to a solution of 0.48 g (0.0015 mole) of ethyl 1-cyclopropyl-6,7-difluoro-8-methoxy-1,4-dihydro-4-oxoquinoline-3-carboxylate (XXXII) (prepared as described in Preparation 3) in 20 ml of methanol, and the mixture was allowed to stand at room temperature for 5 hours. The reaction mixture was then acidified by adding concentrated hydrochloric acid to precipitate a crystalline substance, which was collected by filtration to afford 0.34 g of 1-cyclopropyl-6,7-difluoro-8-methoxy-1,4-dihydro-4-oxoquinoline-3-carboxylic acid (IIC) as colorless powdery crystals melting at 184°-185° C.

후처리

  1. customto precipitate a crystalline substance, which
  2. filtrationwas collected by filtration

출처 및 근거

ORD 기록
ord-9334a11bbfb74db68cea9f43dec76a13
출처 데이터셋
uspto-grants-1991_03
특허 번호
US04997943

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