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DMAP催化合成氟苯尼考琥珀酸酯的研究
引用本文:张伟,符华林,姜彪,付强,唐文,周凤.DMAP催化合成氟苯尼考琥珀酸酯的研究[J].黑龙江畜牧兽医,2012(1):114-116,119.
作者姓名:张伟  符华林  姜彪  付强  唐文  周凤
作者单位:四川农业大学动物医学院
基金项目: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%。

关 键 词:DMAP  氟苯尼考琥珀酸酯  正交试验

Catalytic synthesis of florfenicol succinate by using DMAP
ZHANG Wei,FU Hua-lin,JIANG Biao,FU Qiang,TANG Wen,ZHOU Feng.Catalytic synthesis of florfenicol succinate by using DMAP[J].Heilongjiang Animal Science And veterinary Medicine,2012(1):114-116,119.
Authors:ZHANG Wei  FU Hua-lin  JIANG Biao  FU Qiang  TANG Wen  ZHOU Feng
Institution:(College of Veterinary Medicine,Sichuan Agricultural University,Ya’an 625014,China)
Abstract: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 Fl-S was identified by the pH test,melting point test,IR,UV and HPLC analyses.The best synthesis process of Fl-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 florfenicol,succinic anhydride and DMAP was 1∶ 1.2∶ 1.2,with a reaction temperature of 60 ℃,reaction time of 8 h.Under these conditions,Fl-S was successfully synthesized,and the average yield ratio of Fl-S reached 80.75%.
Keywords:DMAP  florfenicol succinate  orthogonal test
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