【摘要】 以对羟基苯甲酸甲酯为原料,经醚化、克莱森酯缩合两步反应制得4,4’-二甲氧基二苯甲酰甲烷。采用4因素3水平正交实验优化醚化条件,单因素实验法考察克莱森酯缩合反应的各种影响因素,得到了较佳的工艺条件:以DMSO和THF为混合溶剂,NaH作催化剂,n(对甲氧基苯乙酮)∶n(对甲氧基苯甲酸甲酯)∶n(氢化钠)=1∶2∶4,反应温度30℃,反应时间90 min,收率达78.2%。应用IR与1H NMR光谱进行了结构表征。更多还原

【Abstract】 4,4′-Dimethoxy-dibenzoylmethane was synthesized starting from methyl p-hydroxybenzoate as raw material covering etherification and claisen condensation.Experiment based upon orthogonal design with four factors and three levels was carried out for optimization of conditions of the etherification.Conditions influencing the result of Claisen condensation were investigated by single factor tests.Experimental results showed the suitable conditions as follows:using DMSO and THF as the mixed solvent and sodium hydride as the catalyst for carrying out the Claisen condensation,n(p-methoxyacetophenone) ∶n(methyl-4-methoxybenzoate) ∶n(sodium hydride) = 1 ∶2 ∶4.reaction temperature 30 ℃,reaction time 90 min.The yield can reach 78.2%.The structures were characterized by IR and 1H NMR spectra.更多还原