Reaktion #86013

Reaktionsgleichung

diethyl 2-benzyloxycarbonylaminomalonate

potassium carbonate

potassium iodide

ethyl 2-chloroacetate

hydrochloric acid

→

title compound

Ausbeute 86.1%

diethyl 2-benzyloxycarbonylamino-2-ethoxycarbonylsuccinate

Ausbeute 86.1%

Lösungsmittel

DMF

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe reaction mixture was cooled
2. 2
   Extraktionthe mixture was extracted with ethyl acetate
3. 3
   Waschenthe extract was washed with saturated brine
4. 4
   Trocknendried over anhydrous magnesium sulfate
5. 5
   SonstigeThe solvent was evaporated under reduced pressure
6. 6
   Sonstigethe residue was crystallized from ethyl acetate/n-hexane

Vorschrift

A suspension of diethyl 2-benzyloxycarbonylaminomalonate (5.0 g), potassium carbonate (2.7 g), potassium iodide (0.27 g), and ethyl 2-chloroacetate (2.6 g) in DMF (50 mL) was stirred at 50° C. for 1 hour. The reaction mixture was cooled, and then poured into diluted hydrochloric acid, the mixture was extracted with ethyl acetate, and the extract was washed with saturated brine, and then dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was crystallized from ethyl acetate/n-hexane to obtain the title compound (5.5 g, yield: 86%) as colorless crystals.

Quelle