HRID1973827

反应详情

EQUATION

反应方程式

HRID 1973827 的结构方程式

PROCEDURE

实验过程

A mixture of 3 parts of 4-(methoxymethyl)-N-phenyl-1-(2-phenylethyl)-4-piperidinamine and 5 parts of butanoic acid, anhydride is stirred and refluxed for 8 hours. The reaction mixture is poured onto water and the whole is alkalized with ammonium hydroxide. The product is extracted with trichloromethane. The extract is washed with water, dried, filtered and evaporated. The oily residue is stirred in 1,1'-oxybisethane with activated charcoal. The latter is filtered off and the filtrate is evaporated. The residue is converted into the ethanedioate salt 2-propanol. The salt is filtered off and crystallized from 2-propanone, yielding 1.7 parts of N-[4-(methoxymethyl)-1-(2-phenylethyl)-4-piperidinyl]-N-phenylbutanamide ethanedioate; mp. 174.2° C.

WORKUP

后处理

  1. temperaturerefluxed for 8 hours
  2. additionThe reaction mixture is poured onto water
  3. extractionThe product is extracted with trichloromethane
  4. washThe extract is washed with water
  5. customdried
  6. filtrationfiltered
  7. customevaporated
  8. stirringThe oily residue is stirred in 1,1'-oxybisethane with activated charcoal
  9. filtrationThe latter is filtered off
  10. customthe filtrate is evaporated
  11. filtrationThe salt is filtered off
  12. customcrystallized from 2-propanone