摘要
苯妥英钠是抗癫痫发作的首选用药。以安息香为原料,经氧化、环缩合、成盐3步反应制得目标化合物。环缩合步骤首次采用4-二甲氨基吡啶为催化剂,在V(正丁醇)∶V(水)=1∶1组成的两相体系中,完成联苯甲酰与尿素的环缩合反应,高效得到苯妥英,然后与10%氢氧化钠乙醇溶液成盐得目标化合物,目标化合物的结构经IR和~1HNMR确证。该合成路线具有操作简单、后处理方便、产品纯度高且产率高等优点,适合工业化生产,总产率为84.96%。
Phenytoin sodium is commonly used as antiepileptic drug.The target compound was synthesized by oxidation,cyclic condensation,and salification reactions with benzoin as the starting material.Benzil was condensed with urea to afford phenytoin by 4-dimethylaminopyridine as catalyst in two-phase system,composed of n-butanol and water(volume ratio 1∶1).The target compound was formed by phenytoin and 10%sodium hydroxide ethanol solution.The target product was confirmed by IR and^1HNMR.The synthetic route was easy to operate and the product was easy to purify with higher purity.The total yield was 84.96%,which was suitable for industrial production.
作者
陈艳君
史海波
刘艳
邵柯妹
蒋梦吉
袁道远
金丽莎
文志强
CHEN Yan-jun;SHI Hai-bo;LIU Yan;SHAO Ke-mei;JIANG Meng-ji;YUAN Dao-yuan;JIN Li-sha;WEN Zhi-qiang(Zhejiang Collaborative Innovation Center for High Value Utilization of Byproducts from Ethylene Project,Ningbo Polytechnic,Ningbo 315800,China;College of Chemical Engineering,Ningbo Polytechnic,Ningbo 315800,China)
出处
《化学试剂》
CAS
北大核心
2020年第9期1108-1111,共4页
Chemical Reagents
基金
浙江省2019年度高校国内访问工程师“校企合作项目”(FG2019041)
浙江省教育厅一般科研项目(Y201941131)
浙江省高等教育“十三五”教学改革研究项目(jg20190724)
宁波职业技术学院校级课题项目(NZ20C001)
2018年浙江省大学生科技创新活动计划项目(2018R459011)。
作者简介
陈艳君(1983-),女,山东临沂人,博士,副教授,主要从事药物合成的研究,E-mail:yjchen@nit.zju.edu.cn。
