第 39 卷第 2 期Vol. 39 No. 2
2009 年 4 月Apr 2009

所属栏目:医药及中间体

苯磺酸催化合成7-羟基-4-甲基香豆素
张芳芳,姜 恒*,宫 红,程月红 (辽宁石油化工大学 化学与材料科学学院,辽宁 抚顺 113001)
摘 要:以苯磺酸作催化剂,乙酰乙酸乙酯和间苯二酚为原料,通过Pechmann缩合反应合成7-羟基-4-甲基香豆素。考察了原料配比、催化剂用量和反应温度对产品收率的影响,得到较适宜的合成条件为:在110℃下,催化剂用量为0.5%(以间苯二酚计,n/n),n(乙酰乙酸乙酯)∶n(间苯二酚)=1.3∶1时,反应21 min,平行实验的平均收率为85.0%。产品结构用IR表征。
关键词:7-羟基-4-甲基香豆素;苯磺酸;Pechmann缩合反应;合成
中图分类号:TQ203.3  文献标识码:A  文章编号:1009-9212(2009)02- 0035-03
Synthesis of 7-Hydroxy-4-methylcoumarin Using Phenyl Sulfonic Acid as Catalyst
ZHANG Fang-fang,JIANG Heng*,GONG Hong,CHENG Yue-hong (College of Chemistry and Materials Science,Liaoning Petrochemical University,Fushun 113001,China)
Abstract:7-Hydroxy-4-methylcoumarin was synthesized from ethyl acetoacetate and m-dihydroxybenzene by the Pechmann condensation using phenyl sulfonic acid as catalyst under solvent-free conditions. Various affecting factors were investigated. When the amount of catalyst was about 0.5%(m-dihydroxybenzene,n/n),the mole ratio of ethyl acetoacetate to m-dihydroxybenzene was 1.3∶1,the yield reached to 85.0% under 110℃ in 21 min. The structure of the product was confirmed by IR.
Key words:7-hydroxy-4-methylcoumarin;phenyl sulfonic acid;Pechmann condensation;synthesis
基金项目:辽宁省教育厅资助项目(2007T108)。
作者简介:张芳芳(1984-),女,山东滨州人,硕士研究生,研究方向:绿色化学与催化。(E-mail:zffabc@163.com)
联 系 人:姜 恒,教授。(E-mail:hjiang78@hotmail.com)
收稿日期:2009-03-17