تفاعل #90750

معادلة التفاعل

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

hydrogen chloride

→

ethyl 2-oxopiperidine-4-carboxylate

المردود 94.5%

المذيبات

DCM

dioxane

ظروف التفاعل

المعالجة

1. 1
   أخرىthe solvent was removed under reduced pressure
2. 2
   workup.DISSOLUTIONThe resulting residue was dissolved in DCM
3. 3
   استخلاصThe mixture was extracted with DCM
4. 4
   غسيلthe combined organic layer was washed with water, brine
5. 5
   تجفيفdried over anhydrous Na2SO4
6. 6
   تركيزThe organic layer was concentrated in vacuo

الإجراء التجريبي

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%).

المصدر