The title compound [Zn（btzb）2Cl2]·2H2O （1·2H2O, btzb = 1,2-bis（5-tetrazolyl）ben- zene） was synthesized in situ by the [2＋3] cycloaddition reaction of phthalonitrile with NaN3 in water in the presence ...The title compound [Zn（btzb）2Cl2]·2H2O （1·2H2O, btzb = 1,2-bis（5-tetrazolyl）ben- zene） was synthesized in situ by the [2＋3] cycloaddition reaction of phthalonitrile with NaN3 in water in the presence of ZnCl2 under refluxing conditions. 1·2H2O crystallizes in the monoclinic system, space group P2 1/c with a = 9.0119（18）, b = 7.5566（15）, c = 18.076（5）A, β= 114.67（2）°, V= 1118.6（4）A^3, Z = 2, Dc = 1.784 g/cm^3, T= 223（2） K, C16H16N16O2Cl2Zn, Mr = 600.74, F（000） = 608, μ（MoKα） = 1.393 mm^-1, S = 1.081, R = 0.0306 and wR = 0.0669 for 1896 observed reflections with I 〉 2σ（I）. The Zn^2＋ ion of 1 is coordinated by four N atoms from two btzb ligands and two Cl atoms, forming a distorted octahedral coordination geometry. A number of intermolecular hydrogen bon- ding interactions between molecules 1 and/or the solvated water molecules result in a 3D hydrogen-bonded structure. The luminescent property of 1·2H2O was also investigated.展开更多
以二甲基亚砜为溶剂,1,4-对二氯苄和吡唑为反应物,微波辐射合成了1,4-二(吡唑基-1-亚甲基)苯。通过实验研究确定最佳合成条件为:微波输出功率为400W、间歇辐射时间为4min、n(吡唑)∶n(对二氯苄)=2.2∶1。最佳条件下产率可达79.6%。经元...以二甲基亚砜为溶剂,1,4-对二氯苄和吡唑为反应物,微波辐射合成了1,4-二(吡唑基-1-亚甲基)苯。通过实验研究确定最佳合成条件为:微波输出功率为400W、间歇辐射时间为4min、n(吡唑)∶n(对二氯苄)=2.2∶1。最佳条件下产率可达79.6%。经元素分析及IR、1 H NMR表征,确认了合成产物结构。展开更多
分别以十二烷基二甲基叔胺、十四烷基二甲基叔胺和对二氯苄(XDC)为原料,"一步法"合成了两种季铵盐双子表面活性剂,通过正交实验优化了合成条件,结果表明,当n(叔胺)∶n(XDC)=2.4∶1、反应温度75℃、反应时间2 h时,XDC转化率达...分别以十二烷基二甲基叔胺、十四烷基二甲基叔胺和对二氯苄(XDC)为原料,"一步法"合成了两种季铵盐双子表面活性剂,通过正交实验优化了合成条件,结果表明,当n(叔胺)∶n(XDC)=2.4∶1、反应温度75℃、反应时间2 h时,XDC转化率达到100%;产物结构经红外光谱(FTIR)、核磁共振氢谱(1HNMR)和碳谱(13CNMR)进行了确认。研究了其表面活性,结果表明:25℃时,碳链长度分别为12和14时,表面活性剂临界胶束浓度(CMC)分别为1.36×10-5和2.56×10^(-6)mol/L,表面张力(γCMC)分别为40.71和35.37 m N/m;p C20值分别为5.63和6.18;表面过剩吸附量(Γmax)分别为2.41×10^(-6)和3.09×10^(-6)mol/m^2;分子最小截面积(Amin)分别为0.69和0.54 nm^2。动态表面张力参数n值分别为0.85、0.74,t*分别为1.05和0.27 s,R1/2分别为14.11和69.79 m N/m/s,R=14的双子表面活性剂的动态表面张力优于R=12时。该季铵盐双子表面活性剂与结构相似的季铵盐表面活性剂如十六烷基三甲基溴化铵(CTAB)相比CMC低2个数量级。展开更多
基金the National Natural Science Foundation of China (No. 20525101)the NSF of Jiangsu Province (No. BK2004205)+1 种基金the Specialized Research Fund for the Doctoral Program of Higher Education (No. 20050285004)State Key Laboratory of Coordination Chemistry
文摘The title compound [Zn（btzb）2Cl2]·2H2O （1·2H2O, btzb = 1,2-bis（5-tetrazolyl）ben- zene） was synthesized in situ by the [2＋3] cycloaddition reaction of phthalonitrile with NaN3 in water in the presence of ZnCl2 under refluxing conditions. 1·2H2O crystallizes in the monoclinic system, space group P2 1/c with a = 9.0119（18）, b = 7.5566（15）, c = 18.076（5）A, β= 114.67（2）°, V= 1118.6（4）A^3, Z = 2, Dc = 1.784 g/cm^3, T= 223（2） K, C16H16N16O2Cl2Zn, Mr = 600.74, F（000） = 608, μ（MoKα） = 1.393 mm^-1, S = 1.081, R = 0.0306 and wR = 0.0669 for 1896 observed reflections with I 〉 2σ（I）. The Zn^2＋ ion of 1 is coordinated by four N atoms from two btzb ligands and two Cl atoms, forming a distorted octahedral coordination geometry. A number of intermolecular hydrogen bon- ding interactions between molecules 1 and/or the solvated water molecules result in a 3D hydrogen-bonded structure. The luminescent property of 1·2H2O was also investigated.
文摘以二甲基亚砜为溶剂,1,4-对二氯苄和吡唑为反应物,微波辐射合成了1,4-二(吡唑基-1-亚甲基)苯。通过实验研究确定最佳合成条件为:微波输出功率为400W、间歇辐射时间为4min、n(吡唑)∶n(对二氯苄)=2.2∶1。最佳条件下产率可达79.6%。经元素分析及IR、1 H NMR表征,确认了合成产物结构。
文摘分别以十二烷基二甲基叔胺、十四烷基二甲基叔胺和对二氯苄(XDC)为原料,"一步法"合成了两种季铵盐双子表面活性剂,通过正交实验优化了合成条件,结果表明,当n(叔胺)∶n(XDC)=2.4∶1、反应温度75℃、反应时间2 h时,XDC转化率达到100%;产物结构经红外光谱(FTIR)、核磁共振氢谱(1HNMR)和碳谱(13CNMR)进行了确认。研究了其表面活性,结果表明:25℃时,碳链长度分别为12和14时,表面活性剂临界胶束浓度(CMC)分别为1.36×10-5和2.56×10^(-6)mol/L,表面张力(γCMC)分别为40.71和35.37 m N/m;p C20值分别为5.63和6.18;表面过剩吸附量(Γmax)分别为2.41×10^(-6)和3.09×10^(-6)mol/m^2;分子最小截面积(Amin)分别为0.69和0.54 nm^2。动态表面张力参数n值分别为0.85、0.74,t*分别为1.05和0.27 s,R1/2分别为14.11和69.79 m N/m/s,R=14的双子表面活性剂的动态表面张力优于R=12时。该季铵盐双子表面活性剂与结构相似的季铵盐表面活性剂如十六烷基三甲基溴化铵(CTAB)相比CMC低2个数量级。
