Реакция #325847

Уравнение реакции

chloroacetyl chloride

4-piperidinecarbonitrile

potassium carbonate

→

title compound

Выход 92.9%

1-(2-chloroacetyl)-4-piperidinecarbonitrile

Выход 92.9%

Растворители

dichloromethane

dichloromethane

Условия реакции

Обработка

1. 1
   Температураwhile maintaining the reaction mixture at −10 to 0° C
2. 2
   workup.ADDITIONAfter the addition
3. 3
   Другоеthe reaction mixture was separated
4. 4
   Экстракцияthe upper aqueous phase was extracted with dichloromethane (2×300 mL)
5. 5
   Концентрированиеthe combined organic phases were concentrated under reduced pressure

Методика

A mixture of 4-piperidinecarbonitrile (200 g, 1.80 mol) and 40% aqueous potassium carbonate solution (342 g, 0.99 mol) in dichloromethane (1 L) was cooled to −10° C., and a solution of chloroacetyl chloride (210 g, 1.86 mol) in dichloromethane (300 mL) was added over about 75 minutes while maintaining the reaction mixture at −10 to 0° C. After the addition was complete, the reaction mixture was separated, the upper aqueous phase was extracted with dichloromethane (2×300 mL), and the combined organic phases were concentrated under reduced pressure to give 312 g of the title compound as a liquid which slowly crystallized on standing. This compound was of sufficient purity to use in subsequent reactions.

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