新人第一帖：求助四氮杂环与乙二醛的反应？

我有个师弟也在做这个哦，你们可以多交流，一定会成为好朋友的

楼主做出来了吗，我有个师弟也在做这个反应，情况和你的差不多。

忘记把文献放上去了，是这个

A methanolic solution of 25 mmol of glyoxal (40% aqueous) was added dropwise, between -5 and 0 ℃, to a cooled methanolic solution of 25 mmol of the tetraazamacrocycle (cyclen, cyclam or homocyclam). The mixture was stirred for 3 h at room temperature. After solvent evaporation, the residue was dissolved in Et2O and the solution filtered to remove polymers. After evaporation of the solvent, bis-aminals were isolated as white solids and used as such in the following steps. 95% yield, mp=94℃（？）
---------New J. Chem., 2001, 25, 1168-1174

您好，可能是溶剂水含量较大，导致没有出现的文献的描述的白色固体。
可能产物本身也极易吸潮，该反应也容易生成聚合物。
可照着溶剂纯化手册将甲醇除水，用新除过水的甲醇下反应，控制好反应时间，然后操作和处理过程尽量避免水的引入。
祝你好运。