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作 者:王银霞 王宏社 Wang Yinxia;Wang Hongshe(Baoji Medical Building Co.,Ltd.,Baoji 721000;College of Chemistry and Chemical Engineering,Baoji University of Arts and Sciences,Baoji 721013,China)
机构地区:[1]宝鸡医药大厦有限责任公司,陕西宝鸡721000 [2]宝鸡文理学院化学化工学院,陕西宝鸡721013
出 处:《广东化工》2020年第12期67-68,共2页Guangdong Chemical Industry
摘 要:7-羟基-4-甲基香豆素是重要的中间体,可以合成医药、农药、香料及染料。本实验在无溶剂条件下合成7-羟基-4-甲基香豆素,催化剂为二正丁基氧化锡(n-Bu2SnO),原料为间苯二酚和乙酰乙酸乙酯。考察了间苯二酚和乙酰乙酸乙酯的摩尔比、催化剂用量、反应温度、反应时间等因素对7-羟基-4-甲基香豆素产率的影响。结果得到较适宜的反应条件是:当苯二酚和乙酰乙酸乙酯的摩尔比为1∶1.2,即间苯二酚的加入量为0.05 mol,乙酰乙酸乙酯的加入量为0.06 mol,催化剂用量为0.62 g,80℃反应1.5 h,7-羟基-4-甲基香豆素的产率为94.3%。7-Hydroxy-4-methyl coumarin is an important intermediate for the synthesis of perfume,medicine,pesticide and dye.7-Hydroxy-4-methyl coumarin was synthesized from resorcinol and ethyl acetoacetate catalyzed by dibutyltin oxide(n-Bu2SnO).The effects of the molar ratio of resorcinol and ethyl acetoacetate,catalyst dosage,reaction time and reaction temperature on the reaction were discussed.The experimental results showed that the optimized reaction conditions for the synthesis of 7-hydroxy-4-methyl coumarin are as follows:when the molar ratio of resorcinol(0.05 mol)to ethyl acetoacetate(0.06 mol)is 1∶1.2,catalyst dosage is 0.62 g,the reaction time is 1.5 h and the reaction temperature is 80℃under solvent-free conditions,the yield of 7-hydroxy-4-methyl coumarin reached 94.3%.
关 键 词:7-羟基-4-甲基香豆素 间苯二酚 乙酰乙酸乙酯 n-Bu2SnO 催化
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