反应详情

0.5 Moles of n-undecyl cyanide and 0.5 moles of diethyl oxalate are mixed in 1,000 ml of dimethylformamide. To this solution is added with ice cooling 0.52 moles of potassium t-butoxide. The mixture is allowed to stir overnight at room temperature. Following evaporation (rotary evaporator under vacuum) of most of the dimethylformamide the residue is mixed with 3 liters of diethyl ether followed by the addition of 1 liter water. The mixture is acidified with concentrated hydrochloric acid to a pH of 3 and then the ether phase is separated. After washing the ether with water and drying the ether over magnesium sulfate evaporation of the ether affords 3-cyano-2-oxotridecanoic acid ethyl ester. Recrystallization from petroleum ether at 30°-60° C. provides pure material.

1. customevaporation (rotary evaporator under vacuum) of most of the dimethylformamide the residue
2. additionis mixed with 3 liters of diethyl ether
3. additionfollowed by the addition of 1 liter water
4. customthe ether phase is separated
5. washAfter washing the ether with water
6. dry with materialdrying the ether
7. customover magnesium sulfate evaporation of the ether