Jin Dong-yuan
2010
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Journal
Chemical Reagents
Abstract
Tert-butyl 2-cyano-2-(4,6-dimethoxypyrimidin-2-yl) acetate was prepared from 2-chloro-4,6-dimethoxypyrimidine and tert-butyl cyanoacetate.2-(4,6-dimethoxypyrimidin-2-yl) acetonitrile was further synthesized using tert-butyl 2-cyano-2-(4,6-dimethoxypyrimidin-2-yl) acetate as raw material and para-toluenesulfonic acid as catalyst via decarboxylic reaction.Effects of reactant composition,reaction temperature and reaction time on the yield of 2-(4,6-dimethoxypyrimidin-2-yl)acetonitrile were investigated,and the optimal conditions were as follows:molar ratio of n[tert-butyl 2-cyano-2-(4,6-dimethoxypyrimidin-2-yl) acetate]∶n(para-toluenesulfonic acid) was around 1∶0.08,reaction temperature was 100 ℃,and reaction time was 2 hours.The yield of 2-(4,6dimethoxypyrimidin-2-yl)acetonitrile was above 90%.Meanwhile,structure of the product was characterized by IR,1HNMR and 13CNMR methods.