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作 者:于雪[1] 柯苗 徐小娜 YU Xue;KE Miao;XU Xiao-na(School of Pharmaceutical&Chemical Engineering,Xianyang Vocational Technical College,Xianyang 712000,China)
机构地区:[1]咸阳职业技术学院医药化工学院,陕西咸阳712000
出 处:《化学工程师》2022年第9期14-16,71,共4页Chemical Engineer
基 金:陕西省自然科学基础研究计划(面上)项目(2022JM-561);咸阳职业技术学院博士科研基金项目(No.2021BK01);咸阳职业技术学院科学研究基金资助项目(No.2020KJB02)。
摘 要:本研究报道了二茂铁甲胺的合成方法。以邻苯二甲酰亚胺为原料,依次经历Mannich反应、傅-克烷基化反应和肼解等3步反应得到目标化合物。中间体及产物其结构经1H NMR和MS(ESI)表征。并分别对影响傅-克烷基化反应和肼解反应的条件进行考察,确定合成二茂铁甲基异吲哚啉-1,3-二酮(4)的适宜反应条件为:物料比为n_(二茂铁∶n2-羟甲基吲哚啉-1,3-二酮)=1.1∶1、三氟化硼乙醚溶液为催化剂;确定合成产物二茂铁甲胺的适宜反应条件为:反应溶剂为水合肼、反应温度为100℃、反应时间3h。The synthetic method for ferrocene methylamine is reported in this paper.Using phthalimide as raw material,the target compound was obtained by Mannich reaction,Friedel-crafts alkylation and hydrazolysis reaction.The structures of the intermediates and product were characterized by 1H NMR and MS(ESI).The suitable reaction conditions for synthesizing ferrocene methylisoindoline-1,3-dione(4)were determined as follows:the material mole ratio of _(n ferrocene∶n2-hydroxymethylisoindoline-1,3-dione)=1.1∶1,ethyl ether boron fluoride solution as catalyst;The optimum reaction conditions for the synthesized ferrocene methylamine were as follows:hydrazine hydrate as the reaction solvent,the reaction was at 100℃for 3h.
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