反应详情

An amount of 19.2 g. (0.15 moles) of pipecolamide is added portionwise to 102 g. (1.0 moles) of acetic anhydride over a 15 minute period with stirring. The temperature rises to ca. 60°C. The mixture is then heated to reflux, during which the solid dissolves and the solution turns a dark brown. After refluxing for 4 hours, the reaction mixture is subjected to vacuum distillation (first at 60 mm Hg to remove acetic acid and excess acetic anhydride, and then at 1-4 mm Hg pressure). Thus is obtained 15.3 grams of 1-acetyl-2-cyanopiperidine, boiling at 104°-14°C. This corresponds to a 67% yield based on pipecolamide.

1. customrises to ca. 60°C
2. temperatureThe mixture is then heated
3. temperatureto reflux, during which the solid
4. dissolutiondissolves
5. temperatureAfter refluxing for 4 hours
6. distillationthe reaction mixture is subjected to vacuum distillation (first at 60 mm Hg
7. customto remove acetic acid and excess acetic anhydride