반응 #90750

반응 방정식

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

hydrogen chloride

→

ethyl 2-oxopiperidine-4-carboxylate

수율 94.5%

용매

DCM

dioxane

반응 조건

후처리

1. 1
   기타the solvent was removed under reduced pressure
2. 2
   workup.DISSOLUTIONThe resulting residue was dissolved in DCM
3. 3
   추출The mixture was extracted with DCM
4. 4
   세척the combined organic layer was washed with water, brine
5. 5
   건조dried over anhydrous Na2SO4
6. 6
   농축The organic layer was concentrated in vacuo

실험 절차

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%).

출처