乙酸香茅酯的绿色合成与结构表征

以香茅醇与乙酸酐为原料, 以NaHSO₄·SiO₂为负载型固体催化剂,采用微波辐射的方式绿色合成乙酸香茅酯.分别考察催化剂中NaHSO₄的质量分数、反应时间、原料用量比、催化剂用量、反应温度、微波辐射功率等因素对酯收率的影响,并采用傅里叶变换红外光谱(FT-IR)和核磁共振氢谱(¹H NMR)确定产物的结构.结果表明:合成乙酸香茅酯的最佳条件为NaHSO₄质量分数为40%,n(酸酐)∶n(醇)=1

Green Synthesis and Structure Characterization of Citronellyl Acetate

Citronellyl acetate was synthesized from citronellol and acetic anhydride by using NaHSO₄·SiO₂ as supported catalyst and under microwave radiation condition. And the optimum reaction conditions such as the loading of NaHSO₄ on SiO₂, the time of microwave radiation, the ratio of the feeds, the quantity of the catalyst, the reaction temperature and the power of microwave radiation were studied. The results showed that the optimum technological conditions were as following: the loading of NaHSO₄ 40%, the ration of acetic anhydride and citronellyl 1.4∶1, the radiation time 9 minutes, the quantity of catalyst 20%, the reaction temperature 70 ℃, the microwave power 480 W. Under the optimum conditions, the yield of the citronellyl acetate was up to 98.3%. The structure of citronellyl acetate was characterized by FT-IR and ¹H NMR spectra. Furthermore, NaHSO₄·SiO₂ could be recycled and reused at least 4 times and still displayed satisfied catalytic activity.