2-氯乙基乙基醚的无溶剂合成

Solvent-free synthesis of 2-chloroethyl ethyl ether

摘要:

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反应，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2-氯乙基乙基醚，并采用1H-NMR和GC-MS对产物结构进行了表征。采用单因素实验研究了投料摩尔比例、反应温度和反应时间对产物色谱纯度和收率的影响。优化后，投料摩尔比例为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4 h。在此工艺下经公斤级中试放大，产品的收率可达90.2%以上、色谱纯度达到99.4%以上、含量达到99.2%以上。

Abstract:

The solvent-free synthesis process of 2-chloroethyl ethyl ether was improved. Using triethylamine as the catalyst for the reaction of 2-ethoxyethanol with thionyl chloride, the obtained product was washed with saturated sodium bicarbonate solution, saturated sodium chloride solution and dried with anhydrous sodium sulfate to obtain 2-chloroethyl ethyl ether. The structure of product was characterized by 1H-NMR and GC-MS. The effects of molar ratio of reactants, reaction temperature and reaction time on the chromatographic purity and yield of the product were investigated by one-variable at-a-time optimization approach. After optimization, the molar ratio of 2-ethoxyethanol : thionyl chloride : triethylamine was set to 1.0 : 1.3 : 0.3, the reaction temperature was 70 °C, and the reaction time was 4 h. Under this process, the product yield over 90.2% and the chromatographic purity over 99.4%，the assay over 99.2% were obtained after pilot-scale amplification of kilograms.