Synthesis and Crystal Structure of 3,9-Bis(pyridin-2-yl)-2,4,8,10-tetraoxaspiro[5.5]undecane |
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引用本文: | 李正义,葛玲,陈亮,汤秋征,靳琳琳,孙小强.Synthesis and Crystal Structure of 3,9-Bis(pyridin-2-yl)-2,4,8,10-tetraoxaspiro[5.5]undecane[J].结构化学,2012(5):728-732. |
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作者姓名: | 李正义 葛玲 陈亮 汤秋征 靳琳琳 孙小强 |
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作者单位: | Key Laboratory of Fine Petrochemical Engineering, Changzhou University, Changzhou 213164, China |
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基金项目: | supported by the National Natural Science Foundation of China (No. 20872051 and 21002009); the Scientific and Technological Project of Changzhou (CJ20115019); the Priority Academic Program Development of Jiangsu Higher Education Institutions |
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摘 要: | The title compound 3,9-bis(pyridin-2-yl)-2,4,8,10-tetraoxaspiro5.5]undecane 4(C17H18N2O4) has been synthesized by the reaction of 2,2-bis(hydroxymethyl)propane-1,3-diol with pyridine-2-carbaldehyde in the presence of p-toluenesulfonic acid,and characterized by IR,1H-NMR and X-ray single-crystal diffraction.The crystal belongs to monoclinic system,space group C2/c with a = 25.133(2),b = 5.7219(5),c = 21.942(2) ,β = 99.145(2)°,V = 3115.3(5)3,Z = 8,Dc = 1.340 g/cm3,Mr = 314.33,F(000) = 1328,μ = 0.097 mm-1,MoKa radiation(λ = 0.71073),R = 0.0352 and wR = 0.1022 for 2486 observed reflections with I > 2σ(I).X-ray analysis reveals that the two 1,3-dioxane rings passing through the central spiro-C atom both adopt chair conformation.Intermolecular C-H…π,C-H…O and C-H…N weak interactions link the molecules to form a three-dimensional samdwich,which are effective in the stabilization of the crystal structure.
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关 键 词: | spiro-1 3-dioxane 2 2-bis(hydroxymethyl)propane-1 3-diol diacetal synthesis crystal structure |
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