反应详情

温度

25 °C

With stirring, a solution of phenylacetylene (10.2 g) in dioxane (10 ml), a solution of piperidine (13.3 g) in dioxane (10 ml) and copper(I) chloride (0.1 g) were added successively to a suspension of paraformaldehyde (3.6 g) in dioxane (10 ml). The mixture was heated under reflux for 6 hours, allowed to cool to 25° C. and acidified using 20% strength hydrochloric acid. The solution was washed with diethyl ether and the aqueous phase was made alkaline using 50% strength aqueous sodium hydroxide solution and extracted with diethyl ether (3×100 ml). The organic phase was dried with magnesium sulfate and concentrated completely. Distillation of the residue under reduced pressure gave an oil (13.0 g) of boiling point 95° C./0.045 mm Hg.

1. temperatureThe mixture was heated
2. temperatureunder reflux for 6 hours
3. washThe solution was washed with diethyl ether
4. extractionextracted with diethyl ether (3×100 ml)
5. dry with materialThe organic phase was dried with magnesium sulfate
6. concentrationconcentrated completely
7. distillationDistillation of the residue under reduced pressure