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

HRID 1870441

Reaktionsgleichung

Reaktionsgleichung von HRID 1870441
[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

Komponenten

6

Edukt 4

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

Produkt 1

HCID 180010564-Phenyl-1-(4-cyanophenyl)piperidineAusbeute 48,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 13603N-Methyl-2-piperidoneLösungsmittel

Reaktionsbedingungen

Temperatur
20 °C

Versuchsvorschrift

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 1 20° 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.

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-6e029872348445c89b600ee2eba86e16
Quelldatensatz
uspto-grants-2000_08
Patentnummer
US06096735

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