反应详情

To a stirred and cooled mixture of ethyl 4-oxo-1-piperidinecarboxylate (85.5 g), nitromethane (33.6 g) in methanol (240 ml), sodium methoxide (10 g) is added dropwise. Upon completion, stirring is continued for 2 hours at about 10° C. and further overnight at room temperature. The reaction mixture is evaporated at room temperature, crushed ice is added to the oily residue and the whole is acidified with acetic acid. The product is extracted with trichloromethane, the extract is dried, filtered and evaporated. The oily residue solidifies on triturating in petroleumether. The product is filtered off and dried, yielding 73 g of ethyl 4-hydroxy-4-(nitromethyl)-1-piperidinecarboxylate (interm. 5).

1. temperaturecooled
2. additionis added dropwise
3. stirringUpon completion, stirring
4. customThe reaction mixture is evaporated at room temperature
5. customcrushed ice
6. additionis added to the oily residue
7. extractionThe product is extracted with trichloromethane
8. customthe extract is dried
9. filtrationfiltered
10. customevaporated
11. customon triturating in petroleumether
12. filtrationThe product is filtered off
13. customdried