Reaktion #90750

Reaktionsgleichung

1-tert-butyl 4-ethyl 2-oxopiperidine-1,4-dicarboxylate

hydrogen chloride

→

ethyl 2-oxopiperidine-4-carboxylate

Ausbeute 94.5%

Lösungsmittel

DCM

dioxane

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigethe solvent was removed under reduced pressure
2. 2
   workup.DISSOLUTIONThe resulting residue was dissolved in DCM
3. 3
   ExtraktionThe mixture was extracted with DCM
4. 4
   Waschenthe combined organic layer was washed with water, brine
5. 5
   Trocknendried over anhydrous Na2SO4
6. 6
   EinengenThe organic layer was concentrated in vacuo

Vorschrift

To a solution of the 1-tert-butyl 4-ethyl 2-oxopiperidine-1,4-dicarboxylate (20 g, 74.45 mmol) in DCM (93 mL) was add 4N hydrogen chloride in dioxane (30 mL). The reaction was stirred at room temperature for 1 hour and then the solvent was removed under reduced pressure. The resulting residue was dissolved in DCM and water, then adjusted to PH=8 with saturated aqueous Na2CO3 solution. The mixture was extracted with DCM and the combined organic layer was washed with water, brine and dried over anhydrous Na2SO4. The organic layer was concentrated in vacuo to afford ethyl 2-oxopiperidine-4-carboxylate (12 g, yield 94.5%).

Quelle