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Sodium Hydroxide → 1,8-Naphthyridine-3-carboxylic acid, 1-cyclopropyl-6-fluoro-1,4-dihydro-4-oxo-7-(1-piperazinyl)-

HRID 868131
ノート
印刷プレビュー

反応式

HRID 868131 の反応式
[CH:1]1([N:4]2[C:13]3[C:8](=[CH:9][C:10]([F:25])=[C:11]([N:14]4[CH2:19][CH2:18][N:17](C(OCC)=O)[CH2:16][CH2:15]4)[N:12]=3)[C:7](=[O:26])[C:6]([C:27]([O:29]CC)=[O:28])=[CH:5]2)[CH2:3][CH2:2]1.[OH-].[Na+]>C(O)C>[CH:1]1([N:4]2[C:13]3[C:8](=[CH:9][C:10]([F:25])=[C:11]([N:14]4[CH2:15][CH2:16][NH:17][CH2:18][CH2:19]4)[N:12]=3)[C:7](=[O:26])[C:6]([C:27]([OH:29])=[O:28])=[CH:5]2)[CH2:2][CH2:3]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 14798Sodium HydroxideHCID 13565843HCID 13565843、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A suspension of 0.7 g (1.6 mmole) of ethyl 1-cyclopropyl-6-fluoro-1,4-dihydro-4-oxo-7-[4-(ethoxycarbonyl)-1-piperazinyl]-1,8-naphthyridine-3-carboxylate , 6 ml of 10% aqueous sodium hydroxide and 2 ml of ethanol was refluxed for three hours. The reaction was filtered through a fiber glass pad to clarify and acidified to pH 1.5 with 6.0M hydrochloric acid and lyophilized. The residue was dissolved in 10 ml of ammonium hydroxide and the solution concentrated in vacuo. The precipitate which formed was removed by filtration, washed with aqueous ethanol, ether and dried in vacuo to give 0.04 g, mp 274°-276° C.

後処理

  1. temperaturewas refluxed for three hours
  2. filtrationThe reaction was filtered through a fiber glass pad
  3. dissolutionThe residue was dissolved in 10 ml of ammonium hydroxide
  4. concentrationthe solution concentrated in vacuo
  5. customThe precipitate which formed
  6. customwas removed by filtration
  7. washwashed with aqueous ethanol, ether
  8. customdried in vacuo
  9. customto give 0.04 g, mp 274°-276° C.

出典と根拠

ORDレコード
ord-46afaf34c5294bc6a2f52475bf406690
出典データセット
uspto-grants-1988_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04777175

反応ノート

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