反应详情

To start the reaction, a small amount of a solution of 78.1 parts of iodomethane in 70 parts of dry 1,1'-oxybisethane is dropped to a stirred solution of 6.9 parts of lithium in 70 parts of dry 1,1'-oxybisethane. After the addition of 70 parts of dry 1,1'-oxybisethane, the remainder of the solution is added dropwise at reflux temperature. Stirring at reflux is continued for 30 minutes. Then there were added portionwise 16.2 parts of 4-(phenylamino)-1-(2-phenylethyl)-4-piperidinecarboxylic acid (a violent reaction occurs whereby reflux temperature is maintained). Upon completion, stirring at reflux is continued for 1h. 30. The reaction mixture is decomposed by the dropwise addition of 300 parts of water. The organic phase is separated, washed with water, dried, filtered and evaporated. The residue is purified by column-chromatography over silica gel using a mixture of trichloromethane and 5% of methanol as eluent. The first fraction is collected and the eluent is evaporated. The residue is crystallized from 14 parts of 2,2'-oxybispropane, yielding 1-[4-(phenylamino)-1-(2-phenylethyl)-4-piperidinyl]ethanone; mp. 100.6° C.

1. customthe reaction
2. additionthe remainder of the solution is added dropwise
3. temperatureat reflux temperature
4. temperatureat reflux
5. customa violent reaction
6. temperaturereflux temperature
7. temperatureis maintained)
8. stirringUpon completion, stirring
9. temperatureat reflux
10. waitis continued for 1h
11. customThe organic phase is separated
12. washwashed with water
13. customdried
14. filtrationfiltered
15. customevaporated
16. customThe residue is purified by column-chromatography over silica gel using
17. additiona mixture of trichloromethane and 5% of methanol as eluent
18. customThe first fraction is collected
19. customthe eluent is evaporated
20. customThe residue is crystallized from 14 parts of 2,2'-oxybispropane