正交试验优化4-羟基香豆素合成工艺  

Optimization of Synthesis Technology of 4-Hydroxycoumarin by Orthogonal Test

作　　者：朱平华[1,2] 陈文宾[2] 陈连锋[2] 

机构地区：[1]江苏省海洋资源开发研究院,江苏连云港222001 [2]淮海工学院,江苏连云港222005

出　　处：《湖北农业科学》2011年第23期4932-4933,共2页Hubei Agricultural Sciences

基　　金：教育部重点实验室开放基金资助项目(CPEUKF06-04);江苏省自然科学基金企业博士项目(BK2009652);淮海工学院江苏海洋资源开发研究院基金资助项目(JSIMR10C06)

摘　　要：以邻羟基苯乙酮与碳酸二甲酯为原料,氢化钠为缩合剂合成4-羟基香豆素。通过正交试验考察反应温度、反应时间和原料物质的量之比对4-羟基香豆素的影响,结果表明3因素中反应温度对4-羟基香豆素的影响最大,原料物质的量之比的影响最小,最佳反应条件为反应时间1.0 h、原料物质的量之比n邻羟基苯乙酮∶n碳酸二甲酯∶n氢化钠=1.0∶2.0∶1.0、反应温度120℃。在该条件下4-羟基香豆素的产率可达86.6%。4-hydroxycoumarin was synthesized using 2-hydroxyacetophenone and dimethyl carbonate as substrate and sodium hydride as catalytic.Orthogonal test was adopted to analyze the effect of reaction temperature,reaction time and dosage of reactants on the yield of 4-hydroxycoumarin.The result showed that among the three factors,reaction temperature had the most significant effect while dosage of reactants had the lest effect.The optimum reaction conditions were,reaction time,1.0 h;n2-hydroxyacetophenone∶ ndimethyl carbonate∶ nsodium hydride=1.0∶2.0∶1.0;Reaction temperature,120 ℃.The yield of 4-hydroxycoumarin obtained under these conditions was 86.6%.

关 键 词：4-羟基香豆素 合成 正交试验 

分 类 号：O625.45[理学—有机化学]