摘要
以对甲苯磺酸为催化剂、乙酰乙酸乙酯和间苯二酚为原料通过Pechmann反应合成7-羟基-4-甲基香豆素。探讨了以对甲苯磺酸为催化剂时反应温度、催化剂用量、反应时间、原料比诸因素对产品收率的影响。实验表明:对甲苯磺酸是合成7-羟基-4-甲基香豆素的良好催化剂,在反应温度为125℃、反应时间为50min、n(间苯二酚)∶n(三乙)=1∶1.0、催化剂的用量为0.4g(间苯二酚为0.04mol)时,产品收率为65.5%。
7-Hydroxy-4-methyl coumarin was synthesized catalysed by para-toluenesulfonic acid from ethylacetoacetate and resorscinol under solventless condition. The optimum conditions of para-toluene- sulfonic acid were as follows: the molar ratio of ethylacetoacetate to resorscinol was 1:1, the quantity of catalyst was 0.4 gram(when resorscinol was 0.04mol), the reaction temperature was 125℃, and the reaction time was 50min. The yield of 7-hydroxy-4-methyl coumarin could reach 65.5%..
关键词
对甲苯磺酸
香豆素
无溶剂合成
para-toluenesulfonic acid
coumarin
solventless synthesis