摘要
目的:通过超声辅助合成苯妥英,对试验条件进行方法学考察,以确定最佳反应条件。方法:以二苯基乙二酮为原料与尿素在碱性下缩合反应合成苯妥英,设置3因素3水平正交试验与单因素试验对其反应条件进行考察,包括温度、时间、超声功率,筛选出合成反应的最优条件。结果:结合正交试验直观分析和方差分析结果,得出超声合成苯妥英的最佳反应条件为超声功率为80%,超声时间为40 mi,超声温度为75~80℃,在该条件下合成的苯妥英产率为70%。后续的单因素试验结果也进一步验证了该条件的准确性。结论:通过超声合成苯妥英有效地提高产率,且操作简便,与加热回流法相比产率提高34.62%,时间缩短10 min。
Objective:To obtain phenytoin by ultrasound-assisted synthesis,and perform the methodological investigation of experimental conditions to determine the optimum reaction conditions.Methods:In the experiment,phenytoin was synthesized by condensation-assisted reaction of diphenylethylenedione with urea under alkaline condition,and a three-factor-three-level orthogonal test was perfomed.The reaction conditions were investigated,including temperature,time and ultrasonic power,to obtain the optimal conditions for the synthesis reaction.Results:Combined with the orthogonal analysis and analysis of variance results,the optimal reaction conditions for ultrasonic synthesis of phenytoin were as follows:80%ultrasonic power,40 min ultrasonic time and 75-80℃ultrasonic temperature.The subsequent single factor experiment results further validated the accuracy of the conditions.The yield of phenytoin synthesized under the conditions was 70%.Conclusion:The ultrasonic synthesis of phenytoin can effectively shorten the reaction time and is easy to operate.In comparison,the yield increases by 34.62%and the time is shortened by 10 min.
作者
罗家宝
吴艳眉
张泽蓉
罗惠玲
钟桂冬
刘杰润
吴冬兰
陈美先
李艳萍
Luo Jiabao;Wu Yanmei;Zhang Zerong;Luo Huiling;Zhong Guidong;Liu Jierun;Wu Donglan;Chen Meixian;Li Yanping(School of Stomatology(School of Medical Engineering),Foshan University of Science and Technology,Guangdong Foshan 528000,China)
出处
《中国药师》
CAS
2019年第11期2010-2013,共4页
China Pharmacist
基金
佛山市自筹经费类科技计划项目(编号:2018AB003601)
2019年广东大学生科技创新培育专项资金项目(编号:攀登计划pdjh2019b0515)
2019年广东省大学生创新创业训练项目(编号:S201911847075)
关键词
苯妥英
合成工艺
超声辅助
正交试验
Phenytoin
Synthesis process
Ultrasound-assisted
Orthogonal test
作者简介
通讯作者:李艳萍,Tel:(0757)82836985 E-mail:lypfosu@126.com。
