摘要
通过正交试验法优化磷霉素(R)-1-苯乙胺盐的合成工艺。以顺丙烯膦酸为原料,考察了反应温度、催化剂用量、原料物质的量比、反应时间等影响因素对收率的影响,以收率、光学纯度作为综合评价指标,进行正交设计试验,确定最佳合成方案。确定适宜的合成工艺条件为:反应温度65℃、催化剂用量15%、原料物质的量比1∶1、反应时间3 h,在此条件下,磷霉素(R)-1-苯乙胺盐收率达47.3%。催化剂R重复套用5次,其催化活性基本保持一致。验证试验表明:按照正交设计得出的最优方案,制备磷霉素(R)-1-苯乙胺盐的综合收率比现有工艺的收率提高12.3%,并在此基础上解决了催化剂难以回收的问题。
The aim of the present work is to optimize the synthetic process of phosphonomycin(R)-1-phenylethylamine salt by orthogonal design. Here,with cis-propylene phosphoric acid as raw material,the effects of various factors such as reaction temperature,amount of catalyst,reactant molar ratio and reaction time on phosphonomycin(R)-1-phenylethylamine salt yield were investigated. With yield and optical purity as the comprehensive evaluation standard,the optimum experimental scheme was determined by orthogonal design test. The yield of phosphonomycin(R)-1-phenylethylamine salt reaches 47.3% under the optimum synthetic conditions as follows:the reaction temperature of 65 ℃,the amount of catalyst of 15%,the molar ratio of raw material of 1∶1,the reaction time of 3 h. Moreover,the catalytic R is recycled for 5 times,and its catalytic activity is basically consistent. According to the optimal scheme obtained from the orthogonal design,the comprehensive yield of the prepared phosphonomycin(R)-1-phenylethylamine salt increases by 12.3%compared with the existing process,and on this basis,the problem of catalyst recovery is solved.
作者
李雪
金学平
曾祥聪
李爽
李丽
余磊
朱伶俐
周委
祝宏
LI Xue;JIN Xueping;ZENG Xiangcong;LI Shuang;LI Li;YU Lei;ZHU Lingli;ZHOU Wei;ZHU Hong(School of Chemical Engineering and Pharmacy,Wuhan Institute of Technology,Key Laboratory of Green Chemical Process(Wuhan Institute of Technology),Ministry of Education,Hubei Key Laboratory of Novel Chemical Reactor&Green Chemical Technology(Wuhan Institute of Technology),Wuhan 430205,China;Wuhan Drug Solubilization and Delivery Technology Research Center,Wuhan 430205,China;Wuhan Vocational College of Software and Engineering,Wuhan 430205,China)
出处
《武汉工程大学学报》
CAS
2020年第4期390-394,共5页
Journal of Wuhan Institute of Technology
关键词
磷霉素(R)-1-苯乙胺盐
正交设计
顺丙烯膦酸
合成
phosphonomycin(R)-1-phenylethylaminesalt
orthogonaldesign
cis-propylenephosphoricacid
synthesis
