Zhangxin Yu
2010
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Journal
Applied Chemical Industry
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.