3-氰基-3-苯胺基丁酸乙酯的合成研究

以苯甲酰氰为氰化试剂,乙酰乙酸乙酯、苯胺为原料,三组分一锅法合成3-苯胺基-3-氰基丁酸乙酯。重点考察了三组分一锅法中物料配比、反应介质、反应温度和反应时间对产物收率的影响、并通过红外光谱和核磁共振波谱等对产物结构进行了表征。研究结果表明,采用该方法合成3-氰基-3-苯胺基丁酸乙酯的最佳反应条件为:n(苯胺)∶n(乙酰乙酸乙酯)∶n(苯甲酰氰)=1∶1∶1.2,反应介质为二氯甲烷,冰水浴下反应5h,收率达81.5%。

Study on Synthesis of Ethyl 3-cyano-3-anilinobutanoate

Ethyl 3-cyano-3-anilinobutanoate was synthesized from aniline,ethyl acetoacetate and benzoyl cyanide with one pot method.The structure of the target product was confirmed by FT IR,1H NMR and 13C NMR.The effects of reaction medium,reaction temperature and reaction time on the one pot three component reaction were investigated.Under the following optimal reaction conditions: n(aniline)∶n(ethyl acetoacetate)∶n(benzoyl cyanide)=1∶1∶1.2 dichloromethane as reaction medium,and 5 h of reaction time under icy water bathing,the yield of ethyl 3-cyano-3-anilinobutanoate was 81.5%.