二乙二醇甲乙醚的合成

SYNTHESIS OF DIETHYLENE GLYCOL METHYL ETHYL ETHER

以二乙二醇单乙醚(C6H14O3)和氢氧化钠为原料,在n(NaOH):n(C6H14O3)=1.5:1.0,苯为带水剂的条件下,先合成了二乙二醇单乙醚单钠盐,然后使CH3Cl与二乙二醇单乙醚单钠盐进行Williamson反应合成了二乙二醇甲乙醚(DEGMEE)。研究了反应温度、反应时间及CH3Cl/C6H14O3(摩尔比)对DEGMEE收率的影响。用气相色谱法分析了产物的纯度,用FT-IR和1HNMR的方法表征了产物结构。结果表明:在反应温度80℃,CH3Cl通入时间4.0h,n(CH3Cl):n(C6H14O3)=1.40:1的条件下,DEGMEE的收率大于90%。

Diethylene glycol mono-ethyl ether monosodium salt was prepared from diethylene glycol mono-ethyl ether (C6H14O3) and sodium hydroxide with benzene as water carrier under n(NaOH)/n (C6H14O3) = 1. 5 : 1. 0. Then diethylene glycol methyl ethyl ether (DEGMEE) was synthesized through Williamson reaction from CH3Cl and CH3CH2O(CH2CH2O)2Na. The influence of temperature and time of reaction and mass ratio of CH3Cl to diethylene glycol mono-ethyl ether to the yield of DEGMEE was studied. The quality of product was analyzed by GC and the structure of product was characterized by FT-IR and 1 H NMR. The results indicated that the suitable Wiliamson reaction conditions were as follows: reaction temperature 80℃, reaction time 4. 0 h, n(CH3Cl)/n(C6H14 O3) = 1. 4 : 1. The vield of DEGMEE could be more than 90%.