DMAP催化合成氟苯尼考琥珀酸酯的研究  

Catalytic synthesis of florfenicol succinate by using DMAP

作　　者：张伟[1] 符华林[1] 姜彪[1] 付强[1] 唐文[1] 周凤[1] 

机构地区：[1]四川农业大学动物医学院,四川雅安625014

出　　处：《黑龙江畜牧兽医》2012年第1期114-116,119,共4页Heilongjiang Animal Science And veterinary Medicine

基　　金：教育部长江学者和创新团队发展计划创新团队项目(IRT0848)

摘　　要：为了优化氟苯尼考琥珀酸酯(Fl-S)的合成方法并对其进行鉴定,试验以氟苯尼考和琥珀酸酐为原料,4-二甲氨基吡啶(DMAP)为催化剂,丙酮为溶剂,经一步反应合成Fl-S;并以氟苯尼考/DMAP(摩尔比)、氟苯尼考/琥珀酸酐(摩尔比)、反应温度、反应时间为影响因素,选用L9(34)正交试验对合成工艺进行优化;同时分别采用熔点测定法、pH值测定法、红外扫描法、紫外扫描法和高效液相色谱法对Fl-S进行鉴定。结果表明:产物表征符合Fl-S特征;优化的合成条件为氟苯尼考∶琥珀酸酐∶DMAP=1∶1.2∶1.2(摩尔比),反应温度60℃,反应时间8 h。试验成功合成Fl-S,在优化条件下Fl-S平均产率可达80.75%。To optimize the synthesis method of florfenicol succinate （ Fl - S） and identify it. Fl - S was synthesized from florfenicol and succinic anhydride by using 4 - dimethylaminopyridine（DMAP） as a catalyst and acetone as a solvent. The FI -S was identified by the pH test,melting point test,IR,UV and HPLC analyses. The best synthesis process of F1 - S was chosed by a L9 （34 ） orthogonal array design. The results showed that the features of products were consistent with Fl - S. The optimum synthesis conditions were as follows ： the molar ratio among flor- fenicol, succinic anhydride and DMAP was 1：1.2：1.2,with a reaction temperature of 60 ~C ,reaction time of 8 h. Under these conditions, Fl - S was successfully synthesized, and the average yield ratio of Fl -S reached 80.75%.

关 键 词：DMAP 氟苯尼考琥珀酸酯 正交试验 

分 类 号：R931.4[医药卫生—生药学]