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Potassium Carbonate → HCID 20430478、化合物

HRID 2413122
ノート
印刷プレビュー

反応式

HRID 2413122 の反応式
[C:1]([N:4]1[CH2:9][CH2:8][N:7]([C:10]2[N:19]=[C:18]3[C:13]([C:14](=[O:25])[C:15]([C:20]([O:22][CH2:23][CH3:24])=[O:21])=[CH:16][NH:17]3)=[CH:12][C:11]=2[F:26])[CH2:6][CH2:5]1)(=[O:3])[CH3:2].C(=O)([O-])[O-].[K+].[K+].C1(C)C=CC(S(O[CH2:43][CH2:44][F:45])(=O)=O)=CC=1>CN(C)C=O>[C:1]([N:4]1[CH2:9][CH2:8][N:7]([C:10]2[N:19]=[C:18]3[C:13]([C:14](=[O:25])[C:15]([C:20]([O:22][CH2:23][CH3:24])=[O:21])=[CH:16][N:17]3[CH2:43][CH2:44][F:45])=[CH:12][C:11]=2[F:26])[CH2:6][CH2:5]1)(=[O:3])[CH3:2]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 2560192-Fluoroethyl p-ToluenesulfonateHCID 13268404Ethyl 7-(4-acetyl-1-piperazinyl)-6-F-4-hydroxy(1,8)naphthyridine-3-carboxylate

生成物 1

HCID 20430478HCID 20430478、化合物収率 77.6%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
50 °C

実験手順

Ethyl 7-(4-acetyl-1-piperazinyl)-6-fluoro-1,4-dihydro-4-oxo-1,8-naphthyridine-3-carboxylate (7.2 g) and anhydrous potassium carbonate (4.1 g) are added to dimethylformamide (60 ml). The mixture is heated at 50° C. for 30 minutes with stirring. 2-Fluoroethyl p-toluenesulfonate (6.5 g) is added to the mixture, and the mixture is heated at 70°-80° C. with stirring. After the reaction is completed, the insoluble substance is removed by filtration. The filtrate is concentrated to dryness under reduced pressure, and the precipitate is collected by filtration. The precipitate is recrystallized from acetone to give 6.3 g of ethyl 7-(4-acetyl-1-piperazinyl)-6-fluoro-1-(2-fluoroethyl)-1,4-dihydro-4-oxo-1,8-naphthyridine-3-carboxylate (m.p. 183°-185° C.).

後処理

  1. temperaturethe mixture is heated at 70°-80° C.
  2. stirringwith stirring
  3. customthe insoluble substance is removed by filtration
  4. concentrationThe filtrate is concentrated to dryness under reduced pressure
  5. filtrationthe precipitate is collected by filtration
  6. customThe precipitate is recrystallized from acetone

出典と根拠

ORDレコード
ord-669fcbc9544a4b6cb297616487e6302d
出典データセット
uspto-grants-1985_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04496566

反応ノート

読み込み中…

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