反应详情

A mixture of 195.4 parts of potassium hydroxide and 1065 parts of 2-propanol was stirred and warmed till all solid entered solution. After cooling to room temperature, 97 parts of ethyl trans-3-hydroxy-4-[(phenylmethyl)amino]-1-piperidinecarboxylate were added and the whole was stirred and refluxed for 4 hours. The reaction mixture was evaporated to dry and 500 parts of water were added. The whole was concentrated to a volume of about 300 parts. After cooling to room temperature, the product was extracted with dichloromethane. The extract was washed with water, dried, filtered and evaporated. The oily residue was crystallized from acetonitrile. The product was filtered off and dried, yielding 51 parts (70.8%) of trans-4-[(phenylmethyl)amino]-3-piperidinol; mp. 136° C. (intermediate 39).

1. temperaturewarmed till all solid
2. stirringthe whole was stirred
3. temperaturerefluxed for 4 hours
4. customThe reaction mixture was evaporated
5. customto dry
6. addition500 parts of water were added
7. concentrationThe whole was concentrated to a volume of about 300 parts
8. temperatureAfter cooling to room temperature
9. extractionthe product was extracted with dichloromethane
10. washThe extract was washed with water
11. customdried
12. filtrationfiltered
13. customevaporated
14. customThe oily residue was crystallized from acetonitrile
15. filtrationThe product was filtered off
16. customdried