微波辐射一步法合成香料富马酸二苄酯的研究

Synthesis of Benzyl Fumarate by One Step under Microwave Radiation

目的:在微波辐射下,以顺丁烯二酸酐和苄醇为原料,在复合催化剂对甲苯磺酸-硫脲存在下以甲苯为带水剂一步合成了富马酸二苄酯。方法:通过熔点测定和红外光谱分析对产物进行了结构表征。采用正交试验法研究了反应物的摩尔比、催化剂用量、反应温度、辐射反应时间等对产物收率的影响。结果:实验结果表明,在微波功率为700W,n(顺丁烯二酸酸酐):n(苄醇)=1:5,复合催化剂用量为总投料量的7%,甲苯20mL,一酯化、转化、二酯化的温度分别为140℃、145℃、135℃,回流分水90min的条件下,富马酸二苄酯的收率可达92.50%。结论:采用微波辐射法复合催化合成富马酸二苄酯具有操作简便、反应时间短、产物收率高等特点。

Objectives： Benzyl fumarate was synthesized from maleic anhydride and benzyl alcohol under microwave irradiation in one step using toluene as dehydrating agent and 4-methylbenzenesulfonic acid-thiourea as complex catalyst. Methods： Structures of the reaction products were identified by means of melting point measurement and IR spectra. By using an orthogonal test method, the effect of reactants ratio, catalyst dosage, reaction temperature and irradiation time on the product yield was studied. Results： Under optimal reaction conditions： n （maleic anhydride）： n （benzyl alcohol） = 1：5, the complex catalyst dosage was 7% of the totalmass of total feed stock, microwave power 700 W, toluene 20 mL, the temperature of esterification temperature 140, 145 and 135℃, respectively, refluxing and water segrating for 90 min, yield of benzyl fumarate can reach 92.50%. Conclusion： This method had the merits of convenience, short reaction time and high yields.