mPEG5-NHMe与mPEG6-NHMe的合成工艺研究

Synthesis of PEG5-NHMe and PEG6-NHMe

以三乙二醇单甲醚和三乙胺为原料,四氢呋喃作为反应溶剂,经过亲核取代、导入活性离去基团、延长碳链等共4步反应,最终以较好的收率合成了mPEG5-NHMe与mPEG6-NHMe,产物的结构经过~1H NMR确认无误。与之前文献所报道方法相比,产物合成的新路线减少了副反应的发生,降低了分离难度,简化了实验操作的同时也提高了收率。以58. 7%的总收率获得了mPEG5-NHMe,64. 7%的总收率获得了mPEG6-NHMe。

Using three glycol monomethyl ether and triethylamine as raw material, tetrahydrofuran as reactionsolvent, mPEG5-NHMe and mPEG6-NHMe were synthesized with a better yield by a total of 4 steps of reaction such asthe nucleophilic substitution, imported the leaving group activity, extended the carbon chain, etc. The structure ofproducts was confirmed correct by1H NMR. Compared with previous methods reported in the literature, the new methodhad some advantages. It not only reduced the occurrence of side effects, lower the difficulty of separation, but alsoincreased the yield with simplified experimental operations. mPEG5 -NHMe was obtained with a yield of 58. 7%, andmPEG6-NHMe was obtained with a yield of 64.7%.