聚乙二醇单甲醚对甲苯磺酸酯的制备

The synthesis of polyethylene glycol monomethyl ether p-toluene sulfonic acid ester

以相对分子量2 000的聚乙二醇单甲醚(mPEG)与对甲苯磺酰氯(TsCl)为原料,再以三乙胺(TEA)为缚酸剂,进行亲核取代反应制备聚乙二醇单甲醚对甲苯磺酸酯(mPEG-OTs)。运用元素分析检测羟基转化率以及评价反应结果,通过单因素和正交实验来确定不同条件对羟基转化率的影响。结果表明,制备mPEG-OTs最佳工艺为:反应时间12 h,n(mPEG)∶n(TsCl)∶n(TEA)=1∶5.5∶5.5,反应温度为25℃。并通过IR与~1H NMR确定目标产物。

The synthesis of mPEG-OTs was achieved by treatment of the mPEG with TsCl in the solvent of methylene chloride containing TEA which was acid-accepter;and the optimal reaction conditions was obtained by the orthogonal experiment as follow：reaction time was 12 h,mole ratio was n（mPEG）∶n（TsCl）∶n（TEA）=1∶5.5∶5.5 and reaction temperature was 25 ℃;The structures of the product and the intermediate were characterized by means of IR and ~1H NMR,conversion ratio of hydroxyl was obtained by elemental analysis.