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作 者:安敏 贾玮 李明智 An Min;Jia Wei;Li Mingzhi(Xi'an WanLong Pharmaceutical Co.,Ltd.,Shaanxi,Xi'an 710119)
机构地区:[1]西安万隆制药股份有限公司
出 处:《化工与医药工程》2019年第6期6-9,共4页Chemical and Pharmaceutical Engineering
摘 要:以对羟基苯甲酸钠为原料,经醚化、酯化两步反应成功制备4-(2-氨基乙氧基)苯甲酸叔丁醇酯。通过单因素实验考察了合成过程中摩尔比、反应时间、反应温度、干燥时间等工艺参数对反应的影响。适宜工艺为:n(环乙胺)∶n(对羟基苯甲酸钠)=1.3∶1.0、反应时间3~4 h、反应温度50~60℃、干燥时间为5 h,产品总收率为66.1%,纯度98.9%。该合成方法工艺操作简单、反应条件温和,适用于工业化生产,有较好实用价值。The tert-butyl-4-(2-aminoethoxy)benzoate was prepared from the cheap and easily available p-hydroxybenzoic acid sodium salt via etherification and esterification reaction.The influences of experimental parameters,such as the molar ratio of the reactants,reaction time,reaction temperature and drying time on the synthesis were studied by single-factor experiments.It was showed from the preferential experimental results that the optimal reaction condition as follows:the molar ratio of aziridine to p-hydroxybenzoic acid sodium salt is 1.3∶1.0,the reaction time is 3~4 h,reaction temperature is 50~60 degree centigrade,and the drying time is 5 h.The overall yield amounts reached to 66.1% and the purity to 98.9% in the experiment.The improved synthetic process is easy for preparation and needs mild reaction conditions,which is worthful for industrial production and practical application values.
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