反应详情

温度

10 °C

A mixture of 117.7 parts of ethyl 3,4,4-trimethoxy-1-piperidinecarboxylate, 267.3 parts of potassium hydroxide and 720 parts of 2-propanol was stirred and refluxed for 4 hours. The reaction mixture was evaporated. 900 Parts of water were added to the residue and the whole was stirred in a boiling water-bath. The last traces of 2-propanol were removed by evaporation on a Rotavapor. After cooling to 10° C., the product was extracted twice with 280 parts of 1,1'-oxybisethane. The extracts were dried, filtered and evaporated, yielding 62.9 parts (75.4%) of 3,4,4-trimethoxypiperidine as a residue (intermediate 65).

1. temperaturerefluxed for 4 hours
2. customThe reaction mixture was evaporated
3. addition900 Parts of water were added to the residue
4. stirringthe whole was stirred in a boiling water-bath
5. customThe last traces of 2-propanol were removed by evaporation on a Rotavapor
6. extractionthe product was extracted twice with 280 parts of 1,1'-oxybisethane
7. customThe extracts were dried
8. filtrationfiltered
9. customevaporated