反应详情

温度

-10 °C

0.74 g (7.29 mmol) of potassium nitrate are added batchwise at −10° C. to a solution of 1.52 g (6.07 mmol) of N-[4-(2-diethylaminoethoxy)phenyl]acetamide in 25 mL of concentrated sulfuric acid and the mixture is stirred for 1 hour at −10° C. The reaction mixture is poured onto a mixture of ice and concentrated aqueous ammonia and the aqueous phase is exhaustively extracted with ethyl acetate. The combined organic phases are dried over sodium sulfate and evaporated down. Yield: 1.8 g (100% of theory); C14H21N3O4 (M=295.34); calc.: molecular ion peak (M+H)+: 296; found: molecular ion peak (M+H)+: 296; Rf value: 0.50 (Alox, dichloromethane/methanol (39:1)).

1. extractionthe aqueous phase is exhaustively extracted with ethyl acetate
2. dry with materialThe combined organic phases are dried over sodium sulfate
3. customevaporated down