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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
【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%。
【Abstract】 A new organotin oxo cluster compound was synthesized from the reaction of 6-hydroxyl-2-phenyl-3-pyridazinone and di-n-butyltin 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=1.221 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.The identification results show that it has a ladder structure 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%.
【Key words】 tetraorganodistannaxane; hydroxyl-phenyl-pyridazinone; catalitic activity; crystal structure;
- 【文献出处】 应用化学 ,Chinese Journal of Applied Chemistry , 编辑部邮箱 ,2007年12期
- 【分类号】O627.4;O643.36
- 【被引频次】2
- 【下载频次】137