聚乙二醇二羧基醚合成工艺优化  

Optimization of Synthesis Process of Poly(ethylene glycol)bis(carboxymethyl)ether

作　　者：张用芳 米玉伟[2] 刘敏 曾涑源[2] 孙德志[2] ZHANG Yongfang;MI Yuwei;LIU Min;ZENG Suyuan;SUN Dezhi(Institute of BioPharmaceutical Research,Liaocheng University,Liaocheng 252059,China;School of Chemical Engineering and Materials,Liaocheng University,Liaocheng 252059,China)

机构地区：[1]聊城大学生物制药研究院,山东聊城252059 [2]聊城大学化学化工学院,山东聊城252059

出　　处：《聊城大学学报（自然科学版）》2021年第2期89-95,共7页Journal of Liaocheng University:Natural Science Edition

基　　金：国家自然科学基金项目(21473085);山东省抗体制药协同创新中心基金项目(CIC-AD1844);聊城大学博士基金项目(318051916,318051945)资助。

摘　　要：以4-二甲氨基吡啶为催化剂,采用聚乙二醇(PEG,平均分子量为2000 u)和丁二酸酐(SA)反应制得聚乙二醇二羧基醚(PEG-biCOOH)。通过核磁共振氢谱、红外光谱和质谱对所得产品进行了表征。讨论了溶剂、投料配比、反应时间、反应温度对产品收率的影响,优化了PEG-biCOOH的合成工艺。得出最优合成条件为:N,N-二甲基甲酰胺为溶剂,PEG与SA的摩尔比为1∶2.8,反应时间为24 h,反应温度为60℃。此条件下的产物透析后收率较高,为86.7%,为进一步制备药物纳米颗粒、合成前体药物等研究奠定了基础。Poly(ethylene glycol)bis(carboxymethyl)ether(PEG-biCOOH)was successfully prepared with poly(ethylene glycol)(PEG,the average molecular weight is 2000 u)and succinic anhydride(SA)using 4-dimethylaminopyridine as catalyst.The so-obtained product was characterized by 1H-NMR spectra,Fourier transform infrared and Matrix-assisted laser desorption ionization time-of-flight mass spectrometer.The impact of the solvent,the material ratio,time and temperature on yield were determined.This work demonstrates that the optimum reaction conditions are as follows:the solvent is N,N-Dimethylformamide,the molar ratio of PEG to SA is 1:2.8,the reaction time is 24 h,and the reaction temperature is 60℃.The product yield was 86.7%under optimal conditions(after dialysis).It lays a foundation for further research on preparation of drug-nanoparticles and prodrugs.

关 键 词：聚乙二醇 丁二酸酐 聚乙二醇二羧基醚 合成工艺 

分 类 号：O622.5[理学—有机化学]