Title: Synthesis of 3,4-Bis(ethoxycarbonyl)furoxan by One-pot Method
Abstract: 3,4-Bis(ethoxycarbonyl)furoxan was synthesized via nitration,oxidation and cyclization reaction using ethyl acetoacetate as raw material.Its structure was characterized by IR spectrometry and nuclear magnetic resonance(NMR)spectrometry.The reaction mechanism was proposed and the key factors affecting the reaction were studied,as a result,the optimal conditions obtained are as follows:mass fraction of nitric acid,95%;nitration temperature,-10℃;molar ratio of ethyl acetoacetate and nitric acid,1.0∶1.4;molar ratio of catalyst and ethyl acetoacetate,1.0∶100.0;molar ratio of oxidizer and ethyl acetoacetate,3.0∶10.0.Under the optimal conditions,the yield can reach 81.4% and the purity is higher than 98%.
Publication Year: 2015
Publication Date: 2015-01-01
Language: en
Type: article
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