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通过软模剂合成方法合成了高度有序具有二维六方(p6mm)的FDU-15介孔聚合物材料.利用气固相磺化法制备得到新型磺酸基功能化介孔聚合物固体酸(FDU-SO3H).通过X-射线衍射(XRD)、扫描电镜(SEM)及元素分析等测试手段对FDU-SO3H介孔材料的物化性能进行了表征.在无溶剂条件下,FDU-SO3H能有效地催化以芳香醛、乙酰乙酸甲酯和尿素(或硫脲)的三组分一锅法的Biginelli反应.在优化实验的条件下,合成了一系列3,4-二氢嘧啶-2(1H)-酮衍生物.考察了加料顺序、溶剂及反应底物对Biginelli反应的影响.苯甲醛、乙酰乙酸甲酯和尿素在无溶剂,90℃加热1 h的条件下反应,3,4-二氢嘧啶-2(1H)-酮的产率为91%.探讨了Biginelli可能的反应机理.实验结果证明,FDU-SO3H不仅具有催化活性高、对环境友好及在空气中稳定等优点,而且重复使用后仍能保持优异的催化活性.
FDU-15 mesoporous polymer materials with high order and two-dimensional hexagonal structure (p6mm) were synthesized by the method of soft-mold synthesis. A novel sulfonic acid functionalized mesoporous polymer solid acid FDU-SO3H) .The physical and chemical properties of FDU-SO3H mesoporous materials were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and elemental analysis.Under the solvent-free conditions, FDU-SO3H was effective Catalyzed the one-pot Biginelli reaction of aromatic aldehydes, methyl acetoacetate and urea (or thiourea) .A series of 3,4-dihydropyrimidine-2 (1H) ) -ketone derivatives.The effects of the order of addition, solvent and substrate on the reaction of Biginelli were investigated.The reaction of benzaldehyde, methyl acetoacetate and urea in the absence of solvent and heating at 90 ℃ for 1 h, The yield of tetrahydropyrimidin-2 (1H) -one was 91%. The possible reaction mechanism of Biginelli was discussed. The experimental results show that FDU-SO3H not only has the advantages of high catalytic activity, environmental friendliness and stability in the air, After use can still maintain excellent catalytic activity.