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Sulfuric Acid → 7-Chloro-6-fluoro-1-(2,4-difluoro-5-nitrophenyl)-1,4-dihydro-4-oxo-1,8-naphthyridine-3-carboxylic acid

HRID 1415919
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HRID 1415919 반응식
S(=O)(=O)(O)O.[Cl:6][C:7]1[N:16]=[C:15]2[C:10]([C:11](=[O:28])[C:12]([C:25]([OH:27])=[O:26])=[CH:13][N:14]2[C:17]2[CH:22]=[CH:21][C:20]([F:23])=[CH:19][C:18]=2[F:24])=[CH:9][C:8]=1[F:29].[N+:30]([O-])([O-:32])=[O:31].[K+]>>[Cl:6][C:7]1[N:16]=[C:15]2[C:10]([C:11](=[O:28])[C:12]([C:25]([OH:27])=[O:26])=[CH:13][N:14]2[C:17]2[CH:22]=[C:21]([N+:30]([O-:32])=[O:31])[C:20]([F:23])=[CH:19][C:18]=2[F:24])=[CH:9][C:8]=1[F:29]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 1118Sulfuric AcidHCID 24434Potassium NitrateHCID 105460847-Chloro-1-(2,4-difluorophenyl)-6-fluoro-4-oxo-1,4-dihydro-1,8-naphthyridine-3-carboxylic acid

생성물 1

HCID 158603627-Chloro-6-fluoro-1-(2,4-difluoro-5-nitrophenyl)-1,4-dihydro-4-oxo-1,8-naphthyridine-3-carboxylic acid수율 94.7%

실험 절차

To 25 ml of conc. sulfuric acid was added 6.0 grams of 7-chloro-1-(2,4-difluorophenyl)-6-fluoro-4-oxo-1,4-dihydro-1,8-naphthyridine-3-carboxylic acid. With ice cooling and stirring, to the solution was added 5.0 g of potassium nitrate in portions. The temperature was slowly elevated to 80° C. at which stirring was continued for 2 hours. The reaction solution was allowed to cool, poured into 200 g of ice water, and allowed to stand overnight. The precipitate was collected by filtration, washed with distilled water, ethanol and diisopropyl ether, and air dried, to give 6.4 g of the title compound.

후처리

  1. customwas slowly elevated to 80° C. at which
  2. stirringstirring
  3. temperatureto cool
  4. waitto stand overnight
  5. filtrationThe precipitate was collected by filtration
  6. washwashed with distilled water, ethanol and diisopropyl ether, and air
  7. customdried

출처 및 근거

ORD 기록
ord-338745e2cb284a8eb036b86186c1f386
출처 데이터셋
uspto-grants-1999_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05910498

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