摘要
目的研究与优化(7-甲氧基-1-萘基)乙腈的合成工艺,开发适用于工业化生产的简易合成方法。方法以工业级1-氨基-7-萘酚为起始原料,通过重氮化反应、Sandmeyer反应、甲基化反应、偶联反应制得(7-甲氧基-1-萘基)乙腈。对反应温度、时间、反应物配比等因素进行了优化研究,使得该合成反应条件温和,总收率达53.9%。结果与结论中间体与目标化合物结构均经MS和1H NMR确证,优化后的工艺条件温和,适合工业化生产。
Objective To research and optimize the synthesis process of(7-methoxy-1-naphthyl)acetonitrile for industrial production. Methods(7-Methoxy-1-naphthyl)acetonitrile was synthesized from industrial grade 1-amino-7-naphthol,by diazotization,Sandmeyer reaction and coupled reaction. Factors such as the reaction temperature,the reaction time and the ratio of the raw material were optimized to make the reaction conditions mild. The total yield was 53.9%. Results and Conclusion The structures of intermediate and target compounds were confirmed by MS and1 H NMR. The new method is suitable for industrial production.
作者
吴炜
张珩
王莹
杨艺虹
陈红
WU Wei, ZHANG Heng, WANG Ying, YANG Yi-hong, CHEN Hong(School of Chemical Engineering and Pharmacy, Wuhan Institute of Technology, Wuhan 430073, Chin)
出处
《国际药学研究杂志》
CSCD
北大核心
2017年第12期1141-1144,共4页
Journal of International Pharmaceutical Research