Реакция #75609

Уравнение реакции

1-benzyl-4-piperidinecarbonitrile

1-chloroethyl chloroformate

→

4-piperidinecarbonitrile hydrochloride

Растворители

1,2-dichloroethane

Условия реакции

Обработка

1. 1
   Температураunder ice-cooling
2. 2
   Температураheated
3. 3
   Температураunder reflux for 1 hr and 20 min
4. 4
   ДругоеAfter evaporating
5. 5
   workup.ADDITION50 ml methanol was added
6. 6
   Температураit was heated
7. 7
   Температураunder reflux for 1 hr
8. 8
   ДругоеThe reaction solution was evaporated
9. 9
   Промывкаthe crystalline residue was washed with ethyl acetate
10. 10
    Фильтрацияcollected by filtration

Методика

11.0 g of 1-benzyl-4-piperidinecarbonitrile was dissolved in 100 ml 1,2-dichloroethane, 7.1 ml 1-chloroethyl chloroformate was added thereto under ice-cooling. The mixture was stirred at room temperature for 15 min, and then heated under reflux for 1 hr and 20 min. After evaporating, 50 ml methanol was added thereto and it was heated under reflux for 1 hr. The reaction solution was evaporated, and the crystalline residue was washed with ethyl acetate and collected by filtration to give 8.0 g of 4-piperidinecarbonitrile hydrochloride as white crystals.

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