Hydrochloric Acid → 1,8-Naphthyridine-3-carboxylic acid, 1,4-dihydro-7-(3-amino-1-pyrrolidinyl)-1-ethyl-6-fluoro-4-oxo-, monohydrochloride

HRID 1759552노트

반응식

HRID 1759552 반응식
C([NH:4][CH:5]1[CH2:9][CH2:8][N:7]([C:10]2[N:19]=[C:18]3[C:13]([C:14](=[O:25])[C:15]([C:22]([OH:24])=[O:23])=[CH:16][N:17]3[CH2:20][CH3:21])=[CH:12][C:11]=2[F:26])[CH2:6]1)(=O)C.[ClH:27]>>[ClH:27].[NH2:4][CH:5]1[CH2:9][CH2:8][N:7]([C:10]2[N:19]=[C:18]3[C:13]([C:14](=[O:25])[C:15]([C:22]([OH:24])=[O:23])=[CH:16][N:17]3[CH2:20][CH3:21])=[CH:12][C:11]=2[F:26])[CH2:6]1

참가 물질

3

반응물 2

HCID 313Hydrochloric AcidHCID 130411377-[3-(Acetylamino)-1-pyrrolidinyl]-1-ethyl-6-fluoro-1,4-dihydro-4-oxo-1,8-naphthyridine-3-carboxylic acid

생성물 1

HCID 30614691,8-Naphthyridine-3-carboxylic acid, 1,4-dihydro-7-(3-amino-1-pyrrolidinyl)-1-ethyl-6-fluoro-4-oxo-, monohydrochloride

실험 절차

A mixture of 7-(3-acetylamino-1-pyrrolidinyl)-1-ethyl-6-fluoro-1,4-dihydro-4-oxo-1,8-naphthyridine-3-carboxylic acid (1.81 g) in 20% hydrochloric acid (20 ml) was heated under reflux for 3 hours with stirring. The mixture was concentrated to dryness under reduced pressure and then ethanol was added to the residue. After cooling the mixture, the resulting solid was collected and recrystallized from ethanol-water to yield 1.64 g of 7-(3-amino-1-pyrrolidinyl)-1-ethyl-6-fluoro-1,4-dihydro-4-oxo-1,8-naphthyridine-3-carboxylic acid hydrochloride (Compound 1), m.p. 285°-290° C. (decomp.).

후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 3 hours
  3. concentrationThe mixture was concentrated to dryness under reduced pressure
  4. additionethanol was added to the residue
  5. temperatureAfter cooling the mixture
  6. customthe resulting solid was collected
  7. customrecrystallized from ethanol-water

출처 및 근거

ORD 기록
ord-8a131d4acf5448daaa9fa1f1ddb09bd5
출처 데이터셋
uspto-grants-1982_07
특허 번호
US04341784

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