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5-甲氧基-2-[(E)-(吡啶-3-亚氨基)甲基]苯酚的微波固相合成与表征

Microwave Assisted Solid State Synthesis and Character-izations of 5-Methoxy-2-[( E) -( pyridin-3-ylimino) methyl]phenol
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摘要 研究了以2-羟基-4-甲氧基苯甲醛和3-氨基吡啶为原料,微波固相反应合成新型席夫碱衍生物——标题化合物的方法。当2-羟基-4-甲氧基苯甲醛与3-氨基吡啶物质的量比为1.5∶1、反应时间为8 min、微波功率为920 W时,反应产率可达94%以上。用IR、1HNMR、元素分析和X-射线单晶衍射法表征了产物结构。该化合物属正交晶系,空间群为P212121,a=3.940(2),b=10.506(5),c=26.811(14),Dc=1.366 Mg/m3,Z=4,V=1 109.8(10)3,μ=0.094mm-1,R1=0.066 5,wR2=0.106 9。 A new Schiff＇ s base 5-methoxy-2-[（ E）-（ pyridin-3-ylimino） methyl]phenol was synthesized,based on the reaction of 2-hydroxy-4-methoxybenzaldehyde and 3-aminopyridine under microwave irradiation without solvent. Under the optimal reaction conditions,such as microwave power 920 W,reaction time 8 min,1. 5 ∶ 1 molar ratio of 2-hydroxy-4-methoxybenzaldehyde and 3-aminopyridine,the reaction yield was up to 94%. The structure of the product was characterized by IR,UV-Vis,1HNMR and X-ray single crystal diffraction.The compound crystallized in the monoclinic system,space group P212121,with a = 3. 940（ 2） ,b = 10. 506（ 5） ,c =26. 811（ 14） ,Dc= 1. 366 Mg / m3,Z =4,V =1 109. 8（ 10） 3,μ = 0. 094 mm- 1,R1= 0. 066 5,wR2= 0. 106 9.
作者 白林山 周影 王其炎 李竹琴 丁盛 丁举俊
机构地区 安徽工业大学化学与化工学院
出处 《化学试剂》 CAS CSCD 北大核心 2014年第12期1125-1129,共5页 Chemical Reagents
基金 安徽省教育厅自然科学基金资助项目(KJ2012-A050) 安徽省大学生创新创业训练计划基金资助项目(AH201310360143)
关键词 2-羟基-4-甲氧基苯甲醛 3-氨基吡啶 5-甲氧基-2-[(E)-(吡啶-3-亚氨基)甲基]苯酚 席夫碱 微波固相合成 晶体结构 2-hydroxy-4-methoxybenzaldehyde 3-aminopyri-dine 5-methoxy-2-[（E）-（pyridin-3-ylimino）-methyl]phenol Schiff＇ s base microwave assisted solid state synthesis crystal structure
分类号 O621.25 [理学—有机化学]
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参考文献15

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化学试剂
2014年 第12期

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