茴香脑衍生物的合成工艺研究

Study on Synthesis of Anethole Derivatives

以茴香脑为原料经H2O2氧化合成茴香脑环氧化物2-(4-甲氧基苯基)-3-甲基环氧乙烷,产率91%,并研究了溶剂配比、物料配比、催化剂用量、反应温度、反应时间等因素对产物产率的影响。实验结果表明:乙腈与甲醇体积比为1∶5、茴香脑与H2O2的物质的量之比为1∶2.5、原料与无水碳酸钠的物质的量之比为1∶0.8、反应时间为27 h、反应温度为常温时产率最好。茴香脑环氧化物再经氢化铝锂还原得到1-(4-甲氧基苯基)丙-2-醇,并通过单因素试验对其工艺条件进行了优化,初步筛选其优化工艺为:以乙醚为溶剂,原料与还原剂的物质的量之比为1∶1.5,反应温度常温,反应时间1 h。通过GC-MS和IR分析对两种合成物质进行了结构表征。

Epoxidation of anethole with H202 could have 91% yield of 2-（4-methoxyphenyl）-3-methyloxirane. The effects of the ratio of CH3CN/CH3OH, molar ralio of anethole and H202, dosage of catalyst, reaction temperature and reaction time on the yield were investigated. The results showed that the volume of CH3CN/CH3OH was 1 ： 5, the molar ratio of anethole and H202 was 1 ： 2.5, the molar ratio of anethole and anhydrous sodium carbonate was 1 ：0. 8, reaction temperature was room temperature and reaction time was 27 h. Then, reduction of 2-（4-methoxyphenyl）-3-methyloxirane with lithium aluminum hydride was used to obtain 1-（4-methoxyphenyl）-2-propanol. By single factor experiment, the results showed that the optimized conditions were as follows ： ether as the best solvent, molar ratio of raw material to reducing agent was 1 ： 1.5, reaction temperature at room temperature and reaction time 1 h. The structures of the two compounds were characterized by GC-MS and IR.