3-硝酸酯甲基-3-乙基氧杂环丁烷的合成及表征

Synthesis and Characterization of 3-Nitratomethyl-3-Ethyloxetane

以三羟甲基丙烷和碳酸二乙酯为原料,经环化、硝化两步反应合成出了3–硝酸酯甲基–3–乙基氧杂环丁烷(NIMEO),硝化反应的收率为75.1%,产品质量分数为98.8%。通过红外光谱、核磁共振氢谱及元素分析对产品的结构进行了表征,表明为目标化合物。考察了反应条件对产品收率的影响,确定了最佳的硝化条件:硝酸/醋酐为硝化剂,硝化剂与3–羟甲基–3–乙基氧杂环丁烷(HMEO)的摩尔比为1.5∶1.0,反应温度为–10℃,滴加完毕后待温度开始下降时立即中和终止反应。

The 3-nitratomethyl-3-ethyloxetane（NIMEO） was synthesized by two-step reaction of cyclization and nitration using trimethylolpropane and diethyl carbonate as raw materials.The yield of nitration reaction is 75.1%,the product mass fraction is 98.8%.The product structure was characterized by IR,1H-NMR and element analysis.The results show that it is the target product.The effects of reaction conditions on product yield were investigated and the optimum nitrating conditions are fixed as follows：using nitric acid/ acetic anhydride as nitrating agent,n（HNO3）：n（HMEO）=1.5：1.0,reaction temperature of –10℃.The reaction is terminated immediately when the temperature starts to decrease after dropping the reactant to end.