反应详情

温度

60 °C

A mixture of N-(2-amino-1-cyano-2-oxoethyl)-2,6-dimethylisonicotinamide (1.5 g, 0.00646 mol, 1 eq), sodium hydrogen sulfide hydride (1.05 g, 0.00646 mol, 3 eq) in water/1,4-dioxane, diethyl amine hydrochloride (1.0 g, 0.01939 mol, 3 eq) is stirred for 14 h at 60° C. After the completion of the reaction, the reaction mass is allowed to cool, water is added and extracted with ethyl acetate and dried over sodium sulfate. The solvent is evaporated and the crude is recrystallised in diethyl ether to afford 1.0 g of N-(1,3-diamino-1-oxo-3-thioxopropan-2-yl)-2,6-dimethylisonicotinamide; yield: 64%; MS (ESI+): 267;

1. customAfter the completion of the reaction
2. temperatureto cool
3. extractionextracted with ethyl acetate
4. dry with materialdried over sodium sulfate
5. customThe solvent is evaporated
6. customthe crude is recrystallised in diethyl ether