两种色酮膦酸酯类化合物的合成及其结构表征  

Synthesis and structural characterization of two chromone phosphonate derivatives

作　　者：王俊岭[1] 冯书晓[1] 汪小伟[1] 吴峰敏[1] 谷广娜 马军营[1] WANG Jun-ling;FENG Shu-xiao;WANG Xiao-wei;WU Feng-min;GU Guang-na;MA Jun-ying(Chemical Engineering and Pharmaceutics College,Henan University of Science and Technology,Luoyang 471003,China)

机构地区：[1]河南科技大学化工与制药学院,河南洛阳471023

出　　处：《化学研究与应用》2022年第2期268-273,共6页Chemical Research and Application

摘　　要：在超声波辐射下,以3-甲酰基色酮,对硝基苯胺和亚磷酸酯为原料,“一锅法”合成了两种含色酮环的α-氨基膦酸酯类化合物,通过IR,^(1)H NMR,^(13)C NMR,^(31)P NMR,ESI-MS对其结构进行了测定和表征。对化合物4a进行了X射线衍射分析,O,O′-二乙基-α-对硝基苯氨基-α-(色酮-4-基)-甲基膦酸酯(4a)(CCDC:2080073)晶体属单斜晶系,C2/c空间群,晶胞参数为a=33.6146(11)Å,b=12.7607(4)Å,c=20.5344(4)Å,β=90.943(3)°,V=8806.9(4)Å^(3),Z=16,C_(21)H_(27)N_(4)O_(3)P,Mr=432.36,D_(c)=1.304g·cm^(-3),μ=1.484,F(000)=3616,μ(Cu_(Kα))=1.54184 mm^(-1)。An ultrasound promoted efficient,environment friendly process had been devised for the synthesis of two novelα-aminophosphonates through a one-pot three-component condensation of 3-formylchromone,p-nitroaniline and two different types dialkyl phosphate.The desired products were obtained in excellent yields and in high purity under solvent-free and catalyst-free conditions.Their structures were confirmed by IR,LC-MS and ^(1)H NMR The crystal structure of compounds 4a(CCDC:2080073)was also determined by single-crystal X-ray diffraction.It crystallized in monoclinic system,space group C2/c with a=33.6146(11)Å,b=12.7607(4)Å,c=20.5344(4)Å,β=90.943(3)°,V=8806.9(4)Å3,Z=16,C_(20)H_(21)N_(2)O_(7)P,Mr=432.36,D_(c)=1.304g·cm^(-3),μ=1.484,F(000)=3616.0,Cu_(Kα) radiation(λ=1.54184Å).

关 键 词：Α-氨基膦酸酯 色酮 晶体结构 合成 

分 类 号：O626[理学—有机化学]