摘要
研究以氰乙酸甲酯和一氯甲烷为起始原料,经三步反应合成得到2,2-二甲基丙二腈。氰乙酸甲酯在碳酸钾存在条件下,与一氯甲烷甲基化反应生成2-氰基-2-甲基丙酸甲酯;2-氰基-2-甲基丙酸甲酯与氨气氨解反应生成2-氰基-2-甲基丙酰胺;2-氰基-2-甲基丙酰胺在氯化亚砜条件下脱水反应生成2,2-二甲基丙二腈。通过工艺条件优化,最终产品总收率为42.3%,纯度为99.0%,目标产物采用核磁共振对产品进行结构表征。
A new method of synthesizing 2,2-dimethylmalononitrile was studied from cyanoacetate and methyl chloride through three steps.Methyl cyanoacetate reacted with methyl chloride in the presence of potassium carbonateto produce methyl 2-cyano-2-methylpropanoate;methyl 2-cyano-2-methylpropanoate reacted with ammonia gas to produces 2-cyano-2-methylpropanamide;2-cyano-2-methylpropanoyl reacted with thionyl chloride to produce 2,2-dimethylmalononitrile.Through optimization of process conditions,the final product total yield was 42.3%and the purity was 99.0%.The structure of the title compound was characterized by 1H NMR,and13C NMR.
作者
林波
徐龙
余威
沈华良
Lin Bo;Xu Long;Yu Wei;Shen Hualiang(Zhejiang HisoarChuannan Pharmaceutical Co. ,Ltd. , Zhejiang Linhai 317000)
出处
《化工时刊》
CAS
2019年第4期14-16,共3页
Chemical Industry Times
