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Nitric Acid → HCID 178524694、化合物

HRID 622569
ノート
印刷プレビュー

反応式

HRID 622569 の反応式
[N+]([O-])(O)=[O:2].[CH:5]1([N:8]2[C:17]3[C:12](=[CH:13][C:14]([F:24])=[C:15](N4CCNCC4)[N:16]=3)[C:11](=[O:25])[C:10]([C:26]([OH:28])=[O:27])=[CH:9]2)[CH2:7][CH2:6]1>S(=O)(=O)(O)O>[CH:5]1([N:8]2[C:17]3[C:12](=[CH:13][C:14]([F:24])=[C:15]([OH:2])[N:16]=3)[C:11](=[O:25])[C:10]([C:26]([OH:28])=[O:27])=[CH:9]2)[CH2:7][CH2:6]1
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 2

HCID 944Nitric AcidHCID 4654511,8-Naphthyridine-3-carboxylic acid, 1-cyclopropyl-6-fluoro-1,4-dihydro-4-oxo-7-(1-piperazinyl)-

生成物 1

HCID 178524694HCID 178524694、化合物

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

実験手順

To a solution of 2 ml of 70% nitric acid in 10 ml of 98% sulfuric acid was added in portions 1.0g (3.0 mmole) of 1-cyclopropyl-6-fluoro-1,4-dihydro-4-oxo-7-(1-piperazinyl)-1,8-naphthyridine-3-carboxylic acid, keeping the temperature between 25°-30° C. The resulting solution was stirred at room temperature for 18 hours and poured onto 40 g of ice. The mixture was stirred at room temperature for 24 hours, concentrated in vacuo, the pH adjusted to 12 with aqueous sodium hydroxide, and filtered through a fiber glass pad. The filtrate was acidified to pH 3.5 with 6.0M hydrochloric acid, the resulting precipitate removed by filtration, washed with water then ether and dried in vacuo to give 0.23 g of the title compound, mp 325°-327° C.

後処理

  1. custombetween 25°-30° C
  2. stirringThe mixture was stirred at room temperature for 24 hours
  3. concentrationconcentrated in vacuo
  4. filtrationfiltered through a fiber glass pad
  5. customthe resulting precipitate removed by filtration
  6. washwashed with water
  7. dry with materialether and dried in vacuo

出典と根拠

ORDレコード
ord-a252a9dd62d142e59bd627ec5fd17e98
出典データセット
uspto-grants-1988_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04771054

反応ノート

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