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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 622567
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HRID 622567 반응식
[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
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참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 13565843HCID 13565843, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-0ffbc023799243e6ac67f4f1a3d93df8
출처 데이터셋
uspto-grants-1988_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04771054

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