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Sodium Carbonate → 1-[(5-Chloro-2-oxo-1,2-dihydro-3-pyridinyl)methyl]-4-[(E)-2-(2-fluorophenyl)-1-ethenyl]piperidine

HRID 1837772
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HRID 1837772 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([CH2:10][N:11]2[CH2:16][CH2:15][CH:14](/[CH:17]=[CH:18]/[C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=3[F:25])[CH2:13][CH2:12]2)[C:5]([O:8]C)=[N:6][CH:7]=1.C(OCC)(=O)C.Cl.C(=O)([O-])[O-].[Na+].[Na+]>C(O)C>[Cl:1][C:2]1[CH:3]=[C:4]([CH2:10][N:11]2[CH2:12][CH2:13][CH:14](/[CH:17]=[CH:18]/[C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=3[F:25])[CH2:15][CH2:16]2)[C:5](=[O:8])[NH:6][CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 10340Sodium CarbonateHCID 21866389Hydrogen chloride-ethyl acetateHCID 226785031-[(5-Chloro-2-methoxy-3-pyridinyl)methyl]-4-[(E)-2-(2-fluorophenyl)-1-ethenyl]piperidine

생성물 1

HCID 98411871-[(5-Chloro-2-oxo-1,2-dihydro-3-pyridinyl)methyl]-4-[(E)-2-(2-fluorophenyl)-1-ethenyl]piperidine수율 49.3%

시약·촉매·용매 1

HCID 702
Ethanol
용매

실험 절차

In ethanol (8 ml) was dissolved 245 mg of 1-[(5-chloro-2-methoxy-3-pyridinyl)methyl]-4-[(E)-2-(2-fluorophenyl)-1-ethenyl]piperidine. To the mixture was added 7 ml of a 4N-hydrogen chloride-ethyl acetate solution, followed by heating under reflux for 7 hours. An aqueous sodium carbonate was added to the reaction solution, and the mixture was extracted with ethyl acetate. The extract was dried over anhydrous magnesium sulfate, and then the solvent was evaporated. Ether was added to the resulting oil to be crystallized, and 116 mg of the title compound was obtained as a slight yellow powder.

후처리

  1. temperatureby heating
  2. temperatureunder reflux for 7 hours
  3. extractionthe mixture was extracted with ethyl acetate
  4. dry with materialThe extract was dried over anhydrous magnesium sulfate
  5. customthe solvent was evaporated
  6. additionEther was added to the resulting oil
  7. customto be crystallized

출처 및 근거

ORD 기록
ord-f33110541bac4ce6a685c00e71523ced
출처 데이터셋
uspto-grants-2004_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06784192B2

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