N,N′-dimethyl-N-(4-pyridyl)-1,2-ethanediamine (DMPE) as a special N-alkylation precursor of 4-dimethylaminopyridine (DMAP) was grafted on the surface of γ-chloropropylated functionalized mesoporous silica MCM-41 to prepare immobilized DMAP. Characterization results of small angle X-ray diffraction, thermogravimetry and derivative thermogravimetry, Fourier transform infrared, scanning electron microscopy, energy-dispersive X-ray and transmission electron microscopy indicated that DMAP was successfully covalently bound to the surface of MCM-41. The highest loading of DMAP reached 0.9 mmol/g, which was 2.5 times higher than that of DMAP immobilized on the normal silica gel. The prepared immobilized DMAP as nucleophilic heterogeneous catalysts was successfully used for the acetylation reaction to produce α-tocopherol acetate. The highest yield reached 90.1% under the optimal condition which was summarized as follows: immobilized DMAP 100 mg, substrates mole ratio (acetic anhydride/α-tocopherol) 3:1, reaction temperature 50 ℃, stirring intensity 500 rpm, reaction in toluene for 12 h. The recyclability and stability of the DMAP grafted MCM-41 were excellent, as demonstrated by its use 20 times during batch operation without any loss of productivity.

将N，N'-二甲基-N-（4-吡啶基）-1,2-乙二胺（DMPE）作为4-二甲基氨基吡啶（DMAP）的特殊N-烷基化前体接枝到γ-氯丙基化的功能化介孔二氧化硅MCM的表面上-41准备固定的DMAP。小角度X射线衍射，热重分析和微分热重分析，傅立叶变换红外光谱，扫描电子显微镜，能量色散X射线和透射电子显微镜的表征结果表明，DMAP已成功地共价结合到MCM-41的表面。DMAP的最高负载达到0.9 mmol / g，比固定在普通硅胶上的DMAP高2.5倍。制备的固定化DMAP作为亲核非均相催化剂已成功用于乙酰化反应以生产α-生育酚乙酸酯。在最佳条件下，最高收率达到90.1％，总结如下：固定化DMAP 100 mg，底物摩尔比（乙酸酐/α-生育酚）3：1，反应温度50℃，搅拌强度500 rpm，在甲苯中反应12小时 DMAP接枝的MCM-41的可回收性和稳定性极佳，如在分批操作过程中使用20次所证明的那样，而没有任何生产力的损失。