新型固体酸催化7-羟基-4-甲基香豆素的无溶剂合成  

Solventless Synthesis of 7-Hydroxy-4-methylcoumarin with Dodecyl Benzene Sulfonic Acid Catalyst

作　　者：秦省 辛秀兰[1] 徐宝财[1] 

机构地区：[1]北京工商大学化学与环境工程学院,北京100037

出　　处：《精细与专用化学品》2007年第21期18-20,26,共4页Fine and Specialty Chemicals

摘　　要：以新型固体酸为催化剂,乙酰乙酸乙酯和间苯二酚为原料,通过Pechmann反应在无溶剂条件下合成了7-羟基-4-甲基香豆素。探讨了以新型固体酸为催化剂时反应温度、催化剂用量、反应时间、原料配比诸因素对产品收率的影响。实验表明,新型固体酸是合成7-羟基-4-甲基香豆素的良好催化剂,在反应温度为120℃,反应时间70min,n(间苯二酚)∶n(乙酰乙酸乙酯)=1∶1.2,催化剂的用量0.9g(间苯二酚的物质的量0.04mol)时,产品的收率为66.5%。Using ethyl acetoacetate and resorcinol as raw materials, dodecyl benzene sulfonic acid as catalyst, 7-hydroxy--4-methylcoumarin was synthesized by Pechmann reaction under solventless condition. When the dodecyl benzene sulfonic acid is used as catalyst the factors such as reaction temperature, dosage of catalyst, reaction time and the ratio of the raw materials influencing on the yield of the product were discussed. The optimum conditions are established as follows： the molar ratio of ethylacetoacetate to resorcinol was 1.2 ： 1 ; the dosage of catalyst was 0.9 gram （ when resorcinol was 0.04 mol） , the reaction temperature was 120℃ , and the reaction time was 70 min. Under the aforementioned conditions, the yield of 7-hydroxy-4-methylcoumarin can reach 66.5%.

关 键 词：香豆素 无溶剂合成 间苯二酚 乙酰乙酸乙酯 

分 类 号：TQ24[化学工程—有机化工]