反応 #86013

反応方程式

diethyl 2-benzyloxycarbonylaminomalonate

potassium carbonate

potassium iodide

ethyl 2-chloroacetate

hydrochloric acid

→

title compound

収率 86.1%

diethyl 2-benzyloxycarbonylamino-2-ethoxycarbonylsuccinate

収率 86.1%

溶媒

DMF

反応条件

後処理

1. 1
   温度The reaction mixture was cooled
2. 2
   抽出the mixture was extracted with ethyl acetate
3. 3
   洗浄the extract was washed with saturated brine
4. 4
   乾燥dried over anhydrous magnesium sulfate
5. 5
   その他The solvent was evaporated under reduced pressure
6. 6
   その他the residue was crystallized from ethyl acetate/n-hexane

実験手順

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.

出典