反応 #58967

反応方程式

4-nitrobenzylamine hydrochloride

ethyl 4-chloro-4-oxobutanoate

sodium hydrogen carbonate

→

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

収率 87.0%

溶媒

ethyl acetate

反応条件

後処理

1. 1
   抽出The reaction mixture was extracted with ethyl acetate
2. 2
   洗浄The organic layer was washed with water
3. 3
   乾燥dried over anhydrous magnesium sulfate
4. 4
   濃縮concentrated
5. 5
   その他Recrystallization of the residue from ethyl acetate-hexane

実験手順

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.

出典