Pentaerythritol diacetals and diketals from aromatic aldehydes,aliphatic aldehydes,α,β-unsaturated aldehydes and ketones were synthesized using methanesulfonic acid as catalyst in cyclohexane under reflux temperatur...Pentaerythritol diacetals and diketals from aromatic aldehydes,aliphatic aldehydes,α,β-unsaturated aldehydes and ketones were synthesized using methanesulfonic acid as catalyst in cyclohexane under reflux temperature.The products were characterized by IR,1H NMR and elemental analysis.The procedure provided a simplified synthetic method under moderate condition in shorter reaction time,which avoids using corrosive catalyst,harmful organic solvent and water separator during the reaction.展开更多
The title compound 3,9-bis（pyridin-2-yl）-2,4,8,10-tetraoxaspiro[5.5]undecane 4（C17H18N2O4） has been synthesized by the reaction of 2,2-bis（hydroxymethyl）propane-1,3-diol with pyridine-2-carbaldehyde in the prese...The title compound 3,9-bis（pyridin-2-yl）-2,4,8,10-tetraoxaspiro[5.5]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）（A°） ,β = 99.145（2）°,V = 3115.3（5）（A°）^3,Z = 8,Dc = 1.340 g/cm^3,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.展开更多
文摘Pentaerythritol diacetals and diketals from aromatic aldehydes,aliphatic aldehydes,α,β-unsaturated aldehydes and ketones were synthesized using methanesulfonic acid as catalyst in cyclohexane under reflux temperature.The products were characterized by IR,1H NMR and elemental analysis.The procedure provided a simplified synthetic method under moderate condition in shorter reaction time,which avoids using corrosive catalyst,harmful organic solvent and water separator during the reaction.
基金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
文摘The title compound 3,9-bis（pyridin-2-yl）-2,4,8,10-tetraoxaspiro[5.5]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）（A°） ,β = 99.145（2）°,V = 3115.3（5）（A°）^3,Z = 8,Dc = 1.340 g/cm^3,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.
