2-硝酰氧基甲基四氢呋喃的绿色合成

Green Synthesis of 2-Nitratomethyltetrahydrofuran

为了开发新型硝酸酯聚醚粘合剂,以2-羟甲基四氢呋喃(HMTHF)为原料,经N2O5硝化合成出了2-硝酰氧基甲基四氢呋喃(NMTHF),收率为90.6%,产品纯度为98.9%,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和纯度的影响,确定了最佳的硝化条件:N2O5为硝化剂,N2O5与HMTHF的摩尔比为1.0∶1.0,反应温度为-10℃,滴加试剂完毕后反应5min立即终止反应。

In order to develop new nitratopolyether binders,2-nitratomethyltetrahydrofuran（NMTHF） was synthesized with2-hydroxymethyltetrahydrofuran（HMTHF）as starting material and dinitrogen pentoxide（N2O5）as nitrating agent with yield of90.6%and purity of 98.9%.The structure of NMTHF was characterized by IR,1 H NMR and element analysis.The effects of synthetic conditions on nitration reaction were discussed.The optimized synthetic conditions are as follows：n（N2O5）∶n（HMTHF）=1.0∶1.0,reaction temperature-10 ℃,and keeping reaction for only 5 min when the CH2Cl2 solvent of HMTHF was dropped over.