HRID1904623

反应详情

EQUATION

反应方程式

HRID 1904623 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
240 °C

PROCEDURE

实验过程

To 8.55 g of 6-(4-chlorophenyl)-1-phenyl-2-piperidone were added 5.58 g of copper cyanide and 14 ml of pyridine, and the mixture was heated with stirring at 240° C. for 19 hours. The mixture was treated with diluted ammonia water, and then extracted with ethyl acetate. The extracts were washed with water, dried and treated with activated charcoal. After removal of charcoal and the solvent, the residue was purified by silica gel column chromatography (solvent; ethyl acetate:n-hexane=1:1 to 3), and recrystallized from a mixture of ethyl acetate and isopropyl ether to give 3.48 g of 6-(4-cyanophenyl)-1-phenyl-2-piperidone as pale yellow prisms.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. extractionextracted with ethyl acetate
  3. washThe extracts were washed with water
  4. customdried
  5. additiontreated with activated charcoal
  6. customAfter removal of charcoal
  7. customthe solvent, the residue was purified by silica gel column chromatography (solvent; ethyl acetate:n-hexane=1:1 to 3)
  8. customrecrystallized from a mixture of ethyl acetate and isopropyl ether