反应详情

A mixture of 183.4 parts of ethyl cis-3-methoxy-4-[(phenylmethyl)amino]-1-piperidinecarboxylate, 144 parts of (chloromethyl)benzene, 85 parts of sodium carbonate and 720 parts of methylbenzene was stirred for 10 days at reflux temperature. The reaction mixture was filtered and the filtrate was washed three times with 400 parts of water, dried, filtered and evaporated. Petroleumether was added. The whole was cooled whereupon the product solidified. It was filtered off and crystallized from petroleumether. The product was filtered off and dried in vacuo at 40° C., yielding 155 parts (64%) of ethyl cis-4-[bis(phenylmethyl)amino]-3-methoxy-1-piperidinecarboxylate; mp. 95.2° C. (int. 46).

1. temperatureat reflux temperature
2. filtrationThe reaction mixture was filtered
3. washthe filtrate was washed three times with 400 parts of water
4. customdried
5. filtrationfiltered
6. customevaporated
7. additionPetroleumether was added
8. temperatureThe whole was cooled whereupon the product
9. filtrationIt was filtered off
10. customcrystallized from petroleumether
11. filtrationThe product was filtered off
12. customdried in vacuo at 40° C.