摘要
4,6-二羟基嘧啶是一种重要的医药中间体,主要应用于医药合成领域。研究了4,6-二羟基嘧啶的制备方法,针对现有的合成工艺产率低、成本高的问题进行优化,以丙二酸二乙酯和甲酰胺为原料,以反应温度、甲酰胺的用量、乙醇钠的用量、反应时间为考察因素作单因素实验,确定最佳的反应条件。优化后的合成工艺条件为:反应温度80℃,反应时间5 h,n(丙二酸二乙酯):n(甲酰胺):n(乙醇钠)=1∶4∶3.5,收率达到88.9%,产品纯度在97%以上。
4,6-Dihydroxypyrimidine is an important pharmaceutical intermediate,mainly used in the field of pharmaceutical synthesis.In this paper,the preparation method of 4,6-dihydroxypyrimidine was studied.Aiming at the problems of low yield and high cost of the existing synthesis process,the synthesis process was optimized.Using diethyl malonate and formamide as raw materials,taking the reaction temperature,the amount of formamide,the amount of sodium ethoxide,and the reaction time as the factors,single factor experiments were carried out,and the optimal reaction conditions were determined as follows:the reaction temperature 80℃,the reaction time 5 h,n(diethyl malonate)∶n(formamide)∶n(sodium ethoxide)=1∶4∶3.5.Under above conditions,the yield reached 88.9%,the purity of the product was above 97%.
作者
侯奕彤
王婉婷
梁海
刘海燕
HOU Yi-tong;WANG Wan-ting;LIANG Hai;LIU Hai-yan(Department of Chemical and Environmental Engineering,Yingkou Institute of Technology,Liaoning Yingkou 115014,China;Ynnovate Sanzheng(Yingkou)Fine Chemicals Co.,Ltd.,Liaoning Yingkou115000,China)
出处
《当代化工》
CAS
2020年第2期268-270,274,共4页
Contemporary Chemical Industry
基金
辽宁省重点研发计划:2018230009
辽宁省工程技术研究中心项目:201802380
营口市博士双创计划项目(011002)
营口理工学院创新团队.
作者简介
侯奕彤(1997-),女,辽宁省辽阳市人,研究方向:应用化学专业;通讯作者:梁海(1987-),男,工程师,硕士,研究方向:精细化工中间体。E-mail:lianghaipost@163.com。
