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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
ノート
印刷プレビュー

反応式

HRID 1415919 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 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

生成物 1

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

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-338745e2cb284a8eb036b86186c1f386
出典データセット
uspto-grants-1999_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05910498

反応ノート

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