单甲氧基聚乙二醇氨基的制备  

Preparation of Monomethoxy Poly(ethylene glycol) Amine

作　　者：陈阳建[1,2] 宋潇达[2] 彭富君 黎晶晶[1] 

机构地区：[1]浙江医药高等专科学校生物与制药学院,浙江宁波315100 [2]中国药科大学生命科学与技术学院,江苏南京210009

出　　处：《精细化工》2015年第4期434-437,480,共5页Fine Chemicals

基　　金：宁波市自然科学基金资助项目(2014A610208);浙江医药高等专科学校校级科研项目(ZPCSR2013003)~~

摘　　要：通过两步反应制备了相对分子质量(简称分子量)为5 000的单甲氧基聚乙二醇氨基(m PEG5k-EDA)。首先以单甲氧基聚乙二醇5 000(m PEG5k)和对甲苯磺酰氯(p-Ts Cl)为原料,反应得到活性中间体m PEG5k-OTs,然后通过与乙二胺的亲核取代反应获得目标产物,并通过正交实验确定了最佳反应条件:m PEG5k-OTs与乙二胺的摩尔比为1∶25、反应温度为80℃和反应时间为24 h。产物和中间体的结构通过IR和1HNMR进行表征,并通过SDS-PAGE碘染色法检测产物分子量的变化情况。结果表明,通过该方法能简便快捷地制备m PEG5k-EDA,在最优实验条件下,目标产物的总收率高达76.8%,且SDS-PAGE检测表明,产物纯度较高,不含交联副产物。Monomethoxy poly（ethylene glycol） amine（m PEG5k-EDA） with a relative molecular mass of 5 000 was prepared by two-step reaction.Monomethoxy poly（ethylene glycol） tosylate（m PEG5kOTs） was first synthesized from monomethoxy poly（ethylene glycol） 5000（m PEG5k） and ptoluenesulfonyl chloride（p-Ts Cl）,and then it reacted with ethylenediamine as nucleophile to obtain the target product.The optimal reaction conditions were obtained by the orthogonal experiment as follows：mole ratio between m PEG5k-OTs and ethylenediamine was 1∶25,reaction temperature was 80℃and reaction time was 24 h.The structures of the product and the intermediate were characterized by means of IR and1 HNMR,and the variation of molecular weight of the product was detected by SDSPAGE iodine staining method.The results show that m PEG5k-EDA was prepared quickly and easily by this method,and the overall yield of the target product could be as high as 76.8% under the optimal experimental conditions.The purity of the target product was proved by SDS-PAGE without any crosslinking by-products.

关 键 词：单甲氧基聚乙二醇氨基 乙二胺 对甲苯磺酰氯 亲核取代 SDS-PAGE碘染色法 医药与日化原料 

分 类 号：O633.1[理学—高分子化学]