Jia Si-yuan
2009
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Journal
Chemical Reagents
Abstract
3,5-Dinitrobenzonitrile was synthesized by the process of nitration,esterification,amination and dehydration using benzoic acid as the starting material.The overall yield of 3,5-dinitrobenzonitrile was 42.9%.The product structure was confirmed by IR,NMR,MS spectra and elemental analysis.Methyl 3,5-dinitrobenzoate was synthesized by the one-pot method of acylation and esterification using methyl alcohol and thionyl chloride as esterification agents in order to increase the yield and reduce pollution.Furthermore,the dehydration reaction was improved by using phosphorus oxychloride as the dehydrating agent.In this improved method,the superfluous phosphorus oxychloride and hydrochloric acid produced during the reaction were distilled and removed to decrease the acidity of system and avoid the hydrolyzation of nitrile.The yield of the dehydration reaction was as high as 94.3%.