Ethyl Acetate → 4-Phenyl-1-(4-cyanophenyl)piperidine

HRID 1249976노트

반응식

HRID 1249976 반응식
[C:1]1([CH:7]2[CH2:12][CH2:11][NH:10][CH2:9][CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.F[C:14]1[CH:21]=[CH:20][C:17]([C:18]#[N:19])=[CH:16][CH:15]=1.C(=O)([O-])[O-].[K+].[K+].C(OCC)(=O)C>CN1CCCCC1=O>[C:1]1([CH:7]2[CH2:8][CH2:9][N:10]([C:14]3[CH:21]=[CH:20][C:17]([C:18]#[N:19])=[CH:16][CH:15]=3)[CH2:11][CH2:12]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

참가 물질

6

반응물 4

HCID 8857Ethyl AcetateHCID 11430Potassium CarbonateHCID 145174-FluorobenzonitrileHCID 698734-Phenylpiperidine

생성물 1

HCID 180010564-Phenyl-1-(4-cyanophenyl)piperidine수율 48.7%

시약·촉매·용매 1

HCID 13603N-Methyl-2-piperidone용매

반응 조건

온도
120 °C

실험 절차

4-Phenylpiperidine (0. 5 g), p-fluorobenzonitrile (0.37 g) and potassium carbonate (0.78 g) are dissolved in N-methylpiperidone (5 ml), and the mixture is stirred at 120° C. for five hours. To the reaction solution is added ethyl acetate (50 ml), and the mixture is washed with water, dried over magnesium sulfate, filtered, and concentrated under reduced pressure. To the resulting residue is added methanol, and the insoluble crystals are collected by filtration, dried under reduced pressure to give 4-phenyl-1-(4-cyanophenyl)piperidine (0.39 g) as white needles.

후처리

  1. washthe mixture is washed with water
  2. dry with materialdried over magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure
  5. additionTo the resulting residue is added methanol
  6. filtrationthe insoluble crystals are collected by filtration
  7. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-409f65a68e0e4f41bbdabf5f34dcaecd
출처 데이터셋
uspto-grants-2002_01
특허 번호
US06335327B1

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