反应详情

To a stirred mixture of 230 parts of potassium hydroxide and 1600 parts of 2-propanol was added 155 parts of ethyl cis-4-[bis(phenylmethyl)amino]-3-methoxy-1-piperidinecarboxylate. The whole was stirred and refluxed for 7 hours. The reaction mixture was evaporated. Water was added and the mixture was evaporated till all traces of 2-propanol were removed. The product was extracted with dichloromethane. The extract was washed twice with a sodium chloride solution in water, dried, filtered and evaporated. The residue was purified by column chromatography over silica gel using a mixture of trichloromethane and methanol, saturated with ammonia, (95:5 by volume) as eluent. The pure fractions were collected and the eluent was evaporated. The residue was taken up in dichloromethane. The solution was washed with a sodium hydroxide solution 5%, dried, filtered and evaporated, yielding 70 parts (55%) of cis-3-methoxy-N,N-bis(phenylmethyl)-4-piperidinamine as a residue (int. 47).

1. temperaturerefluxed for 7 hours
2. customThe reaction mixture was evaporated
3. additionWater was added
4. customthe mixture was evaporated till all traces of 2-propanol
5. customwere removed
6. extractionThe product was extracted with dichloromethane
7. washThe extract was washed twice with a sodium chloride solution in water
8. customdried
9. filtrationfiltered
10. customevaporated
11. customThe residue was purified by column chromatography over silica gel using
12. additiona mixture of trichloromethane and methanol
13. customThe pure fractions were collected
14. customthe eluent was evaporated
15. washThe solution was washed with a sodium hydroxide solution 5%
16. customdried
17. filtrationfiltered
18. customevaporated