反应详情

温度

75 °C

21.8 G. of 3-(p-tert.-amyl-phenyl)-2-methyl-propionaldehyde and 11.3 g. of piperidine are heated at reflux in 15 ml. of toluene in a water-separator under nitrogen gasification until the water-cleavage has been completed (6 hours). Subsequently, there are added dropwise at room temperature with stirring 6.9 g. of formic acid, the temperature rising to 36°-40° C. Then, the mixture is heated to 75° C. for 2 hours, 50 Ml. of 2 N hydrochloric acid are added to the cooled solution. The toluene solution is separated. The aqueous-hydrochloric acid solution is made alkaline with 40 ml. of 6 N sodium hydroxide and the product is extracted with ether. The combined ether extracts are washed with water, dried over sodium sulfate and evaporated. By distillation, there is obtained pure 1-[3-(p-tert.-amyl-phenyl)-2-methyl-propyl]-piperidine having a boiling point of 160° C./0.15 Torr.

1. temperatureat reflux in 15 ml
2. custom(6 hours)
3. additionSubsequently, there are added dropwise at room temperature
4. customrising to 36°-40° C
5. customThe toluene solution is separated
6. extractionof 6 N sodium hydroxide and the product is extracted with ether
7. washThe combined ether extracts are washed with water
8. dry with materialdried over sodium sulfate
9. customevaporated
10. distillationBy distillation