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N-甲基吡咯烷酮硫酸氢盐催化合成7-羟基-4-甲基香豆素
引用本文:滕俊江,乔艳辉,林培喜.N-甲基吡咯烷酮硫酸氢盐催化合成7-羟基-4-甲基香豆素[J].化工进展,2012,31(6):1321-1324.
作者姓名:滕俊江  乔艳辉  林培喜
作者单位:广东石油化工学院化学与生命科学学院,广东 茂名 525000
基金项目:茂名市重点科技计划项目
摘    要:以离子液体N-甲基吡咯烷酮硫酸氢盐为催化剂,通过Pechmann缩合反应于无溶剂条件下合成了7-羟基-4-甲基香豆素,实验表明N-甲基吡咯烷酮硫酸氢盐可重复使用并具有较好的催化活性。在原料摩尔比n(间苯二酚)∶n(乙酰乙酸乙酯)为1∶1.3、催化剂Hnmp]HSO4占反应物料总质量的1.2%、回流反应时间3 h的条件下,产品收率达87.24%,经液相色谱分析纯度大于98.5%。

关 键 词:N-甲基吡咯烷酮  硫酸氢盐  7-羟基-4-甲基香豆素  合成

Synthesis of 7-hydroxy-4-methylcoumarin catalyzed by 1-methyl-2-pyrrolidinone hydrosulfate
TENG Junjiang,QIAO Yanhui,LIN Peixi.Synthesis of 7-hydroxy-4-methylcoumarin catalyzed by 1-methyl-2-pyrrolidinone hydrosulfate[J].Chemical Industry and Engineering Progress,2012,31(6):1321-1324.
Authors:TENG Junjiang  QIAO Yanhui  LIN Peixi
Affiliation:School of Chemistry and Life Science,Guangdong College of Petrochemical Technology, Maoming 525000,Guangdong,China
Abstract:7-Hydroxy-4-methylcoumarin was synthesized by Pechmann reaction using ionic liquid 1-methyl-2-pyrrolidinone hydrosulfate as catalyst without solvent.The results showed that 1-methyl-2-pyrrolidinone hydrosulfate could be reused and exhibited excellent catalytic activity.Under the condition as:n(resorcinol)∶n(ethyl acetoacetate)=1∶1.3,1.2%(percent of total mass of reactants) HSO4,refluxing for 3 h,the yield of 7-hydroxy-4-methylcoumarin is up to 87.24%.Purity of product analyzed by HPLC is above 98.5%.
Keywords:1-methyl-2-pyrrolidinone  hydrosulfate  7-hydroxy-4-methylcoumarin  synthesis
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