二乙二醇甲基丁基醚的合成研究

Synthesis of diethylene glycol butylmethyl ether

在氮气保护下,以二乙二醇单甲醚(C5H12O3,DEGME)和正溴丁烷为(n-C4H9Br)原料,氢氧化钠为催化剂,苯为带水剂,通过Williamson反应合成了二乙二醇甲基丁基醚(DGBME);用正交实验法对合成条件进行了优化,气相色谱法分析了产品中DGBME的含量,FT-IR和1HNMR法表征了产物结构。结果表明,适宜的反应条件为:反应温度80℃,反应时间4 h,n(n-C4H9Br)∶n(DEGME)=1.06∶1,n(NaOH)∶n(DEGME)=1.5∶1.0;在此条件下,DGBME的收率可达92%以上。

Diethylene glycol butylmethyl ether（DGBME）was synthesized through Williamson Reaction with diethylene glycol mono-methyl ether（DEGME）and butyl bromide （n-C4H9Br） as starting materials at the atmosphere of N2,hydrate sodium as catalyst and benzene as water carrier,its synthetic condition was optimized by orthogonal experiment.The content of DGBME was analyzed by gas chromatography,its structure was characterized by FT-IR and^1H NMR.The results of experiment indicated the suitable syn-thetic conditions were as following：reaction temperature was 80℃,reaction time was 4.0h,n（n-C4H9Br）：n（DEGME）=1.06：1and n（NaOH） ：n（DEGME）=1.5：1.0.Under this condition,the yield of DC-BME was above 92%.