反应详情

Cyanoacetic acid (8.6 g., 0.1 mole) was dissolved in 35 ml. of dioxane. 4-Carboethoxypiperidine (15.7 g., 0.1 mole) was added--a precipitate rapidly formed. When one-half was added 10 ml. of water was then admixed and the temperature controlled below 24° C. until complete addition. With ice bath cooling, 37% aqueous formaldehyde (18 g., 0.2 mole) was dripped in over an 8-minute period and the temperature allowed to rise to 29° C. accompanied by vigorous carbon dioxide evolution. Two phases separated and stirring was continued for an additional 12 hours. After concentration in a bath at 45° C. and under reduced pressure, 22.4 g. of an oil resulted. The product was distilled, b.p., 130°-132° C./0.6 mm., yield, 16.3 g.

1. customa precipitate rapidly formed
2. additionWhen one-half was added 10 ml
3. additionthe temperature controlled below 24° C. until complete addition
4. temperatureWith ice bath cooling
5. customwas dripped in over an 8-minute period
6. customto rise to 29° C.
7. customTwo phases separated
8. concentrationAfter concentration in a bath at 45° C.
9. customof an oil resulted
10. distillationThe product was distilled
11. custom130°-132° C./0.6 mm
12. custom, yield