반응 #58967

반응 방정식

4-nitrobenzylamine hydrochloride

ethyl 4-chloro-4-oxobutanoate

sodium hydrogen carbonate

→

ethyl 4-[(4-nitrobenzyl)amino]-4-oxobutanoate

수율 87.0%

용매

ethyl acetate

반응 조건

후처리

1. 1
   추출The reaction mixture was extracted with ethyl acetate
2. 2
   세척The organic layer was washed with water
3. 3
   건조dried over anhydrous magnesium sulfate
4. 4
   농축concentrated
5. 5
   기타Recrystallization of the residue from ethyl acetate-hexane

실험 절차

A mixture of 4-nitrobenzylamine hydrochloride (8.0 g), ethyl 4-chloro-4-oxobutanoate (10.47 g), saturated aqueous sodium hydrogen carbonate (100 ml) and ethyl acetate (100 ml) was stirred at room temperature for 2 hrs. The reaction mixture was extracted with ethyl acetate. The organic layer was washed with water, dried over anhydrous magnesium sulfate, and concentrated. Recrystallization of the residue from ethyl acetate-hexane gave ethyl 4-[(4-nitrobenzyl)amino]-4-oxobutanoate (10.3 g, 87%) as colorless prism crystals. melting point: 104-106° C.

출처