摘要
为了实现邻甲基苯甲酸-1,1-二氰基邻甲基苯甲酯的绿色合成,采用亚铁氰化钾为绿色氰源与邻甲基苯甲酰氯通过一锅两步反应来合成。文中重点考察了原料配比,反应温度、反应溶剂、反应时间等因素对产率的影响。结果表明:当n(邻甲基苯甲酰氯)∶n(亚铁氰化钾)=4∶1,二氯甲烷为反应介质,吡啶为催化剂,反应温度为25℃,反应时间为40 min时,邻甲基苯甲酸-1,1-二氰基邻甲基苯甲酯的产率可达84. 2%,产物结构通过傅里叶变换红外光谱(FT-IR),核磁共振光谱(1H NMR,13C NMR),元素分析进行了表征。合成方法具有环境友好、操作简单、产率高、后处理方便等优点。
In order to achieve the green synthesis of o-methyl benzoic acid-1,1-two Cyano-methyl phenyl ester,the potassium ferrocyanide was used as green cyanide source and o-methyl benzoyl chloride was synthesized by two steps in one pot.The effects of the raw material ratio,reac-tion temperature,reaction time and reaction solvent on the yield were investigated.The result indica-ted:n(o-methyl benzoyl chloriden(potassium ferrocyanide)=4-1,the dichloromethane as sol-vent,pyridine as catalyst,40min of reaction time under25°C,the yield of o-methyl benzoic acid-1,1-two cyano o-methyl benzene methyl ester can reach84.2%.The structures of the prod-ucts were confirmed by IR,elemental analysis,XH NMR and13C NMR spectra.This method has the advantages of eco-friendly,simple work-up procedure,high yield,and convenient post-process-ing.
作者
周立王
毛学荣
赵宙兴
ZHOU Liwang;MAO Xuerong;ZHAO Zhouxing(School of Chemical Engineering, Qinghai University, Xining 810016 , China;Research Institute,Jingchu University of Technology ,Jingmen 448000, China)
出处
《青海大学学报（自然科学版）》
2018年第6期34-38,共5页
Journal of Qinghai University(Natural Science)
基金
青海大学2016年专业核心课程建设项目(2016ZYHXKC09)
湖北省科技厅科技计划项目(B2016269)
荆楚理工学院校级科研项目(QDB201601)
