反应详情

温度

110 °C

A mixture of 10.4 parts of 4-(phenylamino)-1-(2-phenylethyl)-4-piperidinecarboxylic acid, sodium salt and 75 parts of hexamethylphosphoric triamide is stirred and heated at 110° C. for a while. It is cooled to 20° C. and 3.7 parts of 2-bromopropane are added dropwise. After stirring for 4 hours, another 0.37 parts of 2-bromopropane is added dropwise. Upon completion, stirring is continued over week-end at room temperature. The reaction mixture is poured onto 150 parts of water and the product is extracted with methylbenzene. The extract is washed with water, dried, filtered and evaporated. The oily residue is dissolved in 1,1'-oxybisethane. The solution is stirred with activated charcoal. The latter is filtered off and the filtrate is evaporated. The oily residue is crystallized from hexane. The product is filtered off and recrystallized from hexane, yielding 1-methylethyl 4-(phenylamino)-1-(2-phenylethyl)-4-piperidinecarboxylate; mp. 78.5° C.

1. temperatureIt is cooled to 20° C.
2. stirringAfter stirring for 4 hours
3. stirringUpon completion, stirring
4. waitis continued over week-end at room temperature
5. extractionthe product is extracted with methylbenzene
6. washThe extract is washed with water
7. customdried
8. filtrationfiltered
9. customevaporated
10. dissolutionThe oily 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. customThe oily residue is crystallized from hexane
15. filtrationThe product is filtered off
16. customrecrystallized from hexane