تفاعل #94944

معادلة التفاعل

carbon dioxide

Cyanoacetic acid

4-Carboethoxypiperidine

formaldehyde

→

2-(4-Carboethoxy-1-piperidylmethyl)propenenitrile

المذيبات

dioxane

water

ظروف التفاعل

المعالجة

1. 1
   أخرىa precipitate rapidly formed
2. 2
   workup.ADDITIONWhen one-half was added 10 ml
3. 3
   workup.ADDITIONthe temperature controlled below 24° C. until complete addition
4. 4
   درجة الحرارةWith ice bath cooling
5. 5
   أخرىwas dripped in over an 8-minute period
6. 6
   أخرىto rise to 29° C.
7. 7
   أخرىTwo phases separated
8. 8
   تركيزAfter concentration in a bath at 45° C.
9. 9
   أخرىof an oil resulted
10. 10
    workup.DISTILLATIONThe product was distilled
11. 11
    أخرى130°-132° C./0.6 mm
12. 12
    أخرى, yield

الإجراء التجريبي

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.

المصدر