2-氯乙基乙基醚的无溶剂合成

Solvent-free synthesis of 2-chloroethyl ethyl ether

对2-氯乙基乙基醚的合成工艺进行了无溶剂合成改进。以三乙胺为催化剂,乙二醇单乙醚与二氯亚砜发生氯代反应合成了2-氯乙基乙基醚,产物经饱和碳酸钠溶液碱洗、饱和氯化钠溶液水洗、无水硫酸钠干燥,得到2-氯乙基乙基醚,采用^(1)HNMR和GC-MS对产物结构进行了表征。采用单因素实验考察了投料物质的量比、反应温度和反应时间对产物GC纯度和收率的影响。优化后2-氯乙基乙基醚的合成工艺为n(乙二醇单乙醚)∶n(二氯亚砜)∶n(三乙胺)=1.0∶1.3∶0.3、反应温度为70℃、反应时间为4h。在该工艺下经公斤级中试放大,产品的收率可达90.2%以上、GC纯度达到99.4%以上、含量达到99.2%以上。

The solvent-free synthesis process of 2-chloroethyl ethyl ether was improved in this research.Purified 2-chloroethyl ethyl ether was obtained from the reaction of 2-ethoxyethanol and thionyl chloride using triethylamine as catalyst,and a series of washing with saturated sodium bicarbonate solution,saturated sodium chloride solution and drying wi th anhydrous sodium sulfate.The structure of the sample produced was then characterized by^(1)HNMR and GC-MS.The effects of molar ratio of reactants,reaction temperature and reaction time on the GC purity and yield of the product were further investigated via single factor experimental analysis.The optimized synthesis process of 2-chloroethyl ethyl ether was as follows:n(2-ethoxyethanol)∶n(thionyl chloride)∶n(triethylamine)=1.0∶1.3∶0.3,reaction temperature of 70℃,and reaction time of 4 h.Under the above conditions,the yield and GC purity of product was over 90.2%and 99.4%,respectively,and the content was over 99.2%after kilogram scale pilot amplification.