反应详情

0.30 g (2.1 mM) of (-)-2-cyano-2-methylpentanoic acid was dissolved in 3 ml of dry ethanol. To the mixture under stirring, 0.49 g (3.2 mM) of phosphorus oxychloride was added dropwise. After the reaction for 3 hours at 80° C., 6 ml of 1N-sodium carbonate aqueous solution was added, followed by extraction with diethyl ether. The resultant ether solution was dried on anhydrous sodium sulfate, followed by distilling-off of the solvent and distillation to obtain 0.32 g (1.9 mM) of (-)-ethyl 2-cyano-2-methylpentanoate. Yield:90%, b.p.:110° C./22 mmHg, [α]D -3.0 degrees, [α]435 -4.5 degrees, (c1, methanol)

1. customAfter the reaction for 3 hours at 80° C.
2. extractionfollowed by extraction with diethyl ether
3. dry with materialThe resultant ether solution was dried on anhydrous sodium sulfate
4. distillationfollowed by distilling-off of the solvent and distillation