반응 #86021

반응 방정식

diethyl 2-benzyloxycarbonylaminomalonate

potassium carbonate

potassium iodide

isopropyl 2-bromoacetate

hydrochloric acid

→

title compound

수율 102.7%

diethyl 2-benzyloxycarbonylamino-2-(isopropyloxycarbonylmethyl)malonate

수율 102.7%

용매

DMF

반응 조건

후처리

1. 1
   온도The reaction mixture was cooled
2. 2
   추출the mixture was extracted with ethyl acetate
3. 3
   세척the extract was washed with saturated brine
4. 4
   건조dried over anhydrous magnesium sulfate
5. 5
   기타The solvent was evaporated under reduced pressure
6. 6
   기타purification

실험 절차

A suspension of diethyl 2-benzyloxycarbonylaminomalonate (5.0 g), potassium carbonate (2.7 g), potassium iodide (0.32 g), and isopropyl 2-bromoacetate (3.5 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 subjected to silica gel column chromatography, and then purification was performed with n-hexane/ethyl acetate (5:1), to obtain the title compound (6.8 g, yield: 99%) as colorless oil.

출처