摘要
以N-(喹啉-8-基)新戊酰胺和DL-1-苯乙醇为原料,酸酐为添加剂,无水三氯化铁为催化剂,1,2-二氯乙烷为溶剂制备标题化合物,产品结构经1HNMR和13CNMR表征。通过单因素实验,考察添加剂的种类、反应时间、反应温度、催化剂用量、添加剂用量对反应收率的影响,最终确定合成标题化合物的最佳条件为:n(N-(喹啉-8-基)新戊酰胺)∶n(DL-1-苯乙醇)∶n(添加剂)=1∶3∶3,催化剂为20 mol%无水三氯化铁,溶剂为1,2-二氯乙烷,反应温度为140℃、反应时间为24 h,产品收率可达83%。方法原料易得、操作简单、步骤节省,为产品的工业化奠定了基础。
The title compound was prepared by N-(quinolin-8-yl)pivalamide and DL-1-phenylethanol.Anhydride,iron(Ⅲ) chloride(anhydrous)and 1,2-dichloroethane were used as additive,catalyst and solvent,respectively.The structure of the product was confirmed by 1HNMR and 13CNMR.Based on single factor experiments,the effects of anhydride,reaction time,reaction temperature,amount of reaction catalyst and the amount of additive on the yields were investigated.The optimal conditions for the synthesis of the title compound were as follows:n(N-(quinolin-8-yl)pivalamide)∶n(DL-1-phenylethanol)∶n(additive)=1∶3∶3,20 mol% of iron(Ⅲ) chloride and 1,2-dichloroethane as solvent,reaction temperature was 140 ℃,the reaction time was 24 h,the product yield can reach 83%.The method has the advantages of easy availability of raw materials,simple operation,and step saving,and lays a foundation for industrialization of products.
作者
张奥文
牛恬静
徐金娣
刘景辉
胡国勤
ZHANG Ao-wen;NIU Tian-jing;XU Jin-di;LIU Jing-hui;HU Guo-qin(College of Chemical Engineering and Energy,Zhengzhou University,Zhengzhou 450000,China)
出处
《化学试剂》
CAS
北大核心
2020年第2期207-210,共4页
Chemical Reagents
基金
2018年度河南省科技攻关项目(182102210184)。
关键词
喹啉
DL-1-苯乙醇
酸酐
苄基化
铁催化
quinoline
DL-1-phenylethanol
anhydride
benzylation
iron catalyzed
