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Hydrochloric Acid → 1-[(2-Oxo-1,2-dihydro-3-pyridinyl)methyl]-4-[2-(2-methylsulfonylaminophenyl)-2-oxoethyl]piperidine

HRID 1837748
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HRID 1837748 반응식
C[O:2][C:3]1[C:8]([CH2:9][N:10]2[CH2:15][CH2:14][CH:13]([CH2:16][C:17]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=3[NH:25][S:26]([CH3:29])(=[O:28])=[O:27])=[O:18])[CH2:12][CH2:11]2)=[CH:7][CH:6]=[CH:5][N:4]=1.Cl>C(#N)C>[O:2]=[C:3]1[C:8]([CH2:9][N:10]2[CH2:11][CH2:12][CH:13]([CH2:16][C:17]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=3[NH:25][S:26]([CH3:29])(=[O:28])=[O:27])=[O:18])[CH2:14][CH2:15]2)=[CH:7][CH:6]=[CH:5][NH:4]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 226783911-[(2-Methoxy-3-pyridyl)methyl]-4-[2-(2-methylsulfonylaminophenyl)-2-oxoethyl]piperidine

생성물 1

HCID 226783001-[(2-Oxo-1,2-dihydro-3-pyridinyl)methyl]-4-[2-(2-methylsulfonylaminophenyl)-2-oxoethyl]piperidine수율 51.7%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

In acetonitrile (4 ml) were dissolved 90 mg of 1-[(2-methoxy-3-pyridyl)methyl]-4-[2-(2-methanesulfonylaminophenyl)-2-oxoethyl]piperidine obtained in Example 65 and 0.30 ml of concentrated hydrochloric acid, followed by heating under reflux for 5 hours. The solvent was evaporated, and then the residue was dissolved in ethyl acetate and an aqueous 1N sodium hydroxide. The organic layer was separated, washed with brine, and then dried over anhydrous magnesium sulfate. The solvent was evaporated, and the crude product was recrystallized from ethanol, to give 45 mg of the title compound as colorless crystals.

후처리

  1. temperatureby heating
  2. temperatureunder reflux for 5 hours
  3. customThe solvent was evaporated
  4. dissolutionthe residue was dissolved in ethyl acetate
  5. customThe organic layer was separated
  6. washwashed with brine
  7. dry with materialdried over anhydrous magnesium sulfate
  8. customThe solvent was evaporated
  9. customthe crude product was recrystallized from ethanol

출처 및 근거

ORD 기록
ord-3209161db6834257a7466943a4a72ec1
출처 데이터셋
uspto-grants-2004_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06784192B2

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