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

HRID 1249976ノート

反応式

HRID 1249976 の反応式
[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

参加物

6

反応物 4

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

生成物 1

HCID 180010564-Phenyl-1-(4-cyanophenyl)piperidine収率 48.7%

試薬・触媒・溶媒 1

HCID 13603N-Methyl-2-piperidone溶媒

反応条件

温度
120 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-409f65a68e0e4f41bbdabf5f34dcaecd
出典データセット
uspto-grants-2002_01
特許番号
US06335327B1

反応ノート

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