Реакция #63441

ord-bac92c456294430c80daef1d6f3fcce0

Уравнение реакции

N#CN1Cc2ccccc2-c2ccccc2C1
5,7-dihydro-6H-dibenz[c,e]azepine-6-carbonitrile
[C-]#N.[K+]
potassium cyanide
C=CCO
allyl alcohol
C=CCOC(=N)N1Cc2ccccc2-c2ccccc2C1
allyl 5,7-dihydro-6H-dibenz[c,e]azepine-6-carboximidate

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.DISTILLATIONthe allyl alcohol is distilled off
  2. 2
    workup.ADDITIONThe residue is poured onto ice/water
  3. 3
    Экстракцияextracted with methylene chloride
  4. 4
    Промывкаthe combined extracts are washed with water
  5. 5
    Сушкаdried over anhydrous sodium sulphate
  6. 6
    Другоеevaporated

Методика

A mixture of 1.99 g of 5,7-dihydro-6H-dibenz[c,e]azepine-6-carbonitrile, 0.59 g of potassium cyanide and 20 ml of allyl alcohol is stirred at room temperature for 20 hours and thereafter the allyl alcohol is distilled off. The residue is poured onto ice/water and extracted with methylene chloride, and the combined extracts are washed with water, dried over anhydrous sodium sulphate and evaporated. After flash chromatography on silica gel (elutent: ethyl acetate) there is obtained pure allyl 5,7-dihydro-6H-dibenz[c,e]azepine-6-carboximidate as an oil.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04766115uspto-grants-1988_08