6-羟基-2-苯基-3-哒嗪酮四丁基二锡氧烷二聚体的合成、表征和催化性能  

Synthesis,Characterization and Catalyzing Capacity of 6-Hydroxyl-2-phenyl-3-pyridazinone-tetrabutyldistannoxane

作　　者：毛武涛[1] 田来进[1] 郑晓风[1] 尹玲[1] 

机构地区：[1]曲阜师范大学化学科学学院,曲阜273165

出　　处：《应用化学》2007年第12期1368-1373,共6页Chinese Journal of Applied Chemistry

基　　金：山东省自然科学基金(Z2002F01)资助课题

摘　　要：由6-羟基-2-苯基-3-哒嗪酮和二丁基氧化锡合成了新的有机锡氧簇化合物Ⅰ,用元素分析、IR、1H、13C和119Sn NMR表征了其结构。由X射线单晶衍射测定了其晶体结构,该化合物属于三斜晶系,P1空间群,晶体学参数为a=1.221 75(13)nm,b=1.267 90(13)nm,c=1.345 33(14)nm,α=87.168 0(10)°,β=672.265 0(10)°,γ=87.261 0(10)°,V=1.981 4(4)nm3,Z=1,Dc=1.435 g/cm3,μ(MoKα)=0.870 0,F(000)=868。该化合物具有中心对称的梯形结构,锡原子为五配位的三角双锥构型。该化合物催化乙酰乙酸乙酯和甲醇的酯交换的产率为88%、催化丙二酸二甲酯和乙醇的酯交换的产率为90%,但较难催化环己酮和甘油的缩酮反应,产率低于22%。A new organotin oxo cluster compound was synthesized from the reaction of 6-hydroxyl-2-phenyl-3-pyridazinone and di-n-butyhin oxide. The compound was characterized by elemental analysis, IR and X-ray single crystal diffraction. The compound shows a centro-symmetric dimer structure mode belonging to the triclinic space group P1- with a= 1.22175（13） nm, b = 1.26790（13） nm, c= 1.34533（14） nm, α=87. 1680（10）°, β=672.2650（10）°, γ=87.2610（10）°, V= 1.9814（4） nm^3, Z = 1, Dc =1. 435 g/cm^3, μ（MoKα） =0. 8700, F（000） = 868. The identification results show that it has a ladder strue-ture with centric symmetry, in which the tin atom is five-coordinated, forming a distorted trigonal bipyramid.The compound can catalyze the transesterification between acetoacetic ester and methanol with a yield of 88% ;it also catalyzes the transesterification between methylmalonate and ethanol with a yield of 90%. However, it is less effective to catalyze the acetalation between cyclohexanone and propanetriol with a yield of no more than 22%.

关 键 词：四烃基二锡氧烷 羟基苯基哒嗪酮.催化活性 晶体结构 

分 类 号：O627.4[理学—有机化学]