反应详情

温度

22 °C

4-(1-Piperidylmethyl)piperidine (0.05 mole) was dissolved in 17 ml. of dioxane containing cyanoacetic acid (4.25 g., 0.05 mole) by warming and the solution then cooled to 22° C. Over a 9 minute period, 37% aqueous formaldehyde (8.5 g., 0.1 mole) was dripped in. The temperature throughout the addition was 25°-28° C. It was then warmed to 35°-40° C. for carbon dioxide evolution and maintained then for 2 hours. The mixture was stripped at a bath temperature of 60° C./15 mm. to leave approximately 12 g. of an oil. Most dissolved in 150 ml. of ether; the solution was washed twice with water, dried over anhydrous sodium sulfate and the solvent stripped. A nearly colorless oil was obtained, 8.6 g., which gradually solidified on standing at room temperature.

1. temperatureby warming
2. additionThe temperature throughout the addition
3. customwas 25°-28° C
4. temperaturemaintained
5. customThe mixture was stripped at a bath
6. customtemperature of 60° C./15 mm
7. customto leave approximately 12 g
8. dissolutionMost dissolved in 150 ml
9. washthe solution was washed twice with water
10. dry with materialdried over anhydrous sodium sulfate
11. customA nearly colorless oil was obtained
12. customon standing at room temperature