四川轻化工大学学报：自然科学版

氧杂环丁烷化合物，因其具有粘度低、毒性小、挥发性小等特点，引起科研工作者与企业广泛关注与研究，它不仅可以作为阳离子型紫外光固化反应的活性稀释剂，同时也可以作为单体参与反应。本文采用碳酸二乙酯(DEC)与三羟甲基丙烷(TMP)为原料，通过酯交换成环-裂解反应制备3-乙基-3-氧杂丁环甲醇(EHO)，探究了催化剂种类与用量、原料配比等因素对合成EHO的影响，通过对合成工艺进行优化，进一步提高了产物的收率与纯度。研究表明，制备EHO较佳工艺条件为：三羟甲基丙烷用量为0.4 mol时，碳酸二乙酯与三羟甲基丙烷为等摩尔比投料，以甲醇钾为催化剂(用量0.25 g)，溶剂为无水乙醇(用量4 mL)，反应时间5 h。在此反应条件下，EHO收率达85.1%，纯度为97.2%(GC)，并采用核磁氢谱(¹H–NMR)和红外(FTIR)对其结构进行了表征和分析。

Due to the low viscosity,low toxicity and low volatility,oxetane compounds have attracted extensive attention and research of researchers and enterprises.It can be used not only as active diluent of cationic UV curing reaction,but also as monomer to participate in the reaction.In this paper,3-ethyl-3-oxetanemethanol (EHO) has been synthesized via ester exchange to ring-cleavage reaction using trimethylolpropane and diethyl carbonate as raw materials,the types and dosage of catalysts,the ratio of raw materials and other factors that has effects on the synthesis of EHO are studied.Furthermore,the yield and purity of the product are further improved by optimizing the synthesis process.The results show that the optimum conditions for the preparation of EHO are as follows:when the amount of trimethylolpropane is 0.4 mol,the molar ratio of diethyl carbonate to trimethylolpropane is 1.0∶1.0,the amount of potassium methanol used as catalyst is 0.25 g,and the amount of anhydrous ethanol used as solvent is 4 mL,the reaction time is 5 h.Under this condition,the yield of EHO is 85.1%,whose purity is 97.2%(GC),and the structure is characterized by nuclear magnetic hydrogen spectroscopy (¹H-NMR) and infrared spectroscopy (FTIR).