Реакция #75608

ord-96af40e9e890427598b15566fb3e39e9

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураcooling
  2. 2
    ДругоеIt was evaporated
  3. 3
    workup.DISSOLUTIONthe resulting residue was dissolved in ethyl acetate
  4. 4
    Промывкаwashed with aqueous sodium hydroxide and brine
  5. 5
    СушкаAfter drying over anhydrous sodium sulfate, it
  6. 6
    Другоеwas evaporated
  7. 7
    Другоеthe resulting residue was purified by silica gel column chromatography

Методика

5 ml N,N-dimethylformamide was added to a mixture of 12.7 g 1-benzyl-4-piperidine carboxamide and 60 ml phosphorus oxychloride under ice-cooling, and it was stirred at room temperature for 1.5 hr. It was evaporated, and the resulting residue was dissolved in ethyl acetate and washed with aqueous sodium hydroxide and brine. After drying over anhydrous sodium sulfate, it was evaporated, and the resulting residue was purified by silica gel column chromatography to give 11.0 g of 1-benzyl-4-piperidine carbonitrile.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US06699870B2uspto-grants-2004_03