反应详情

温度

180 °C

A mixture of 4.8 parts of 1-[4-(phenylamino)-1-(2-phenylethyl)-4-piperidinyl]ethanone and 15 parts of propanoic acid, anhydride is stirred for 5 hours at 180° C (oil-bath). Stirring is continued overnight, while meantime the mixture is allowed to reach room temperature. The reaction mixture is poured onto ice-water and the whole is alkalized with a concentrated ammonium hydroxide solution. The product is extracted with benzene. The extract is washed twice with water, dried, filtered and evaporated in vacuo. The residue is dissolved in 1,1'-oxybisethane and the solution is stirred with activated charcoal. The latter is filtered off and the filtrate is evaporated. The residue is converted into the ethanedioate salt in 2-propanol. The salt is filtered off and crystallized from 2-propanol, yielding N-[4-acetyl-1-(2-phenylethyl)-4-piperidinyl]-N-phenylpropanamide ethanedioate; mp. 196.8° C.

1. stirringStirring
2. waitis continued overnight, while meantime
3. customto reach room temperature
4. additionThe reaction mixture is poured onto ice-water
5. extractionThe product is extracted with benzene
6. washThe extract is washed twice with water
7. customdried
8. filtrationfiltered
9. customevaporated in vacuo
10. dissolutionThe residue is dissolved in 1,1'-oxybisethane
11. stirringthe solution is stirred with activated charcoal
12. filtrationThe latter is filtered off
13. customthe filtrate is evaporated
14. filtrationThe salt is filtered off
15. customcrystallized from 2-propanol