树枝状聚醚的合成与实验条件探讨

Research on the Synthesis and Reaction Conditions of Dendritic Polyether

以3,5-二羟基苯甲醇和氯化苄为原料,经Willamson醚化反应和卤代反应合成了1-3代以CH2Br为核的树枝状聚醚,并分别用核磁和差示扫描量热仪进行了结构和熔点分析。对比了氯化亚砜、三溴化磷、四溴化碳卤代试剂的卤代效果,以及聚乙二醇-400、18-冠-6为相转移催化剂的催化效果。结果表明,采用Williamson醚化反应可以合成确定结构的1-3代树枝状聚醚,其熔点分别为80℃、107℃、122℃。以四溴化碳为卤化剂,冠醚为催化剂可以得到较高的产物收率。

Dendritic polyethers from the first to the third generation, which benzyl bromine is the core, were synthesized by reaction of Williamson and halogenating reaction. 1H NMR and DSC were used to characterize the structure and melt point of the dendritic polyether, respectively. The halogenated efficiency of thionyl chloride, phosphlrus tribromide and tetrabromomethane were compared, and the catalytic effect of 18-crown-6 and polyglycol 400 were studied. The results show that the melt points of the dendritic polyethers from the first to the third generation are 80℃, 107℃ and 122℃, the yields of dendritic polyether are much higher than that of the others＇ when tetrabromomethane and 18-crown-6 are used.