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Hydrochloric Acid → 5-Fluoro-1-[(6-fluoro-2-naphthyl)methyl]-4-oxo-1,4-dihydroquinoline-3-carboxylic acid

HRID 2088985
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HRID 2088985 반응식
[F:1][C:2]1[CH:11]=[CH:10][CH:9]=[C:8]2[C:3]=1[C:4](=[O:17])[C:5]([C:12]([O:14]CC)=[O:13])=[CH:6][NH:7]2.C(=O)([O-])[O-].[K+].[K+].[I-].[K+].Br[CH2:27][C:28]1[CH:37]=[CH:36][C:35]2[C:30](=[CH:31][CH:32]=[C:33]([F:38])[CH:34]=2)[CH:29]=1.[OH-].[Li+].Cl>CN(C=O)C>[F:1][C:2]1[CH:11]=[CH:10][CH:9]=[C:8]2[C:3]=1[C:4](=[O:17])[C:5]([C:12]([OH:14])=[O:13])=[CH:6][N:7]2[CH2:27][C:28]1[CH:37]=[CH:36][C:35]2[C:30](=[CH:31][CH:32]=[C:33]([F:38])[CH:34]=2)[CH:29]=1
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참가 물질

8

반응물 6

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 4875Potassium IodideHCID 11430Potassium CarbonateHCID 5946332-(Bromomethyl)-6-fluoronaphthaleneHCID 58398097Ethyl 5-fluoro-4-oxo-1,4-dihydroquinoline-3-carboxylate

생성물 1

HCID 46187671
5-Fluoro-1-[(6-fluoro-2-naphthyl)methyl]-4-oxo-1,4-dihydroquinoline-3-carboxylic acid

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
40 °C

실험 절차

To a mixture of ethyl 5-fluoro-4-oxo-1,4-dihydroquinoline-3-carboxylate (0.050 g, 0.21 mmol), potassium carbonate (0.088 g, 0.64 mmol) and potassium iodide (3 mg, 0.02 mmol) was added the above 2-(bromomethyl)-6-fluoronaphthalene in 1 mL of DMF. The reaction was stirred overnight at 40° C. and 1 mL of a saturated aqueous lithium hydroxide solution was then added to the reaction. After stirring for 30 min, the solution was acidified with 4 N HCl and the product was extracted three times with EtOAc. The combined organic layers were dried over sodium sulfate, filtered and concentrated in vacuo. The crude material was purified by reverse phase HPLC to provide the 5-fluoro-1-[(6-fluoro-2-naphthyl)methyl]-4-oxo-1,4-dihydroquinoline-3-carboxylic acid which gave a mass ion (ES+) of 366 for M+H+.

후처리

  1. stirringAfter stirring for 30 min
  2. extractionthe product was extracted three times with EtOAc
  3. dry with materialThe combined organic layers were dried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customThe crude material was purified by reverse phase HPLC

출처 및 근거

ORD 기록
ord-7bed42ae01484949851f3b1a1c04cc91
출처 데이터셋
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08436016B2

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