Wu Su-fang
2012
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Journal
Applied Chemical Industry
Abstract
Under the condition of UV,tetramethyl cyclobutane tetracarboxylate is synthesized by using dimethyl fumarate as the raw material and water as the solvent.Cyclobutanetetracarboxylic acid is obtained after hydrolysis of tetramethyl cyclobutane tetracarboxylate,and then the cyclobutanetetracarboxylic dianhydride is obtained after dehydration.The optimal reaction condition for the cycloaddition reaction,hydrolysis reaction and dehydration reaction were as follows:the yield of tetramethyl cyclobutane tetracarboxylate is up to 96.5% under the condition as the proportion of dimethyl fumarate to water 1∶ 5,the reaction time 20 h and the reaction temperature 10 ℃;the yield of cyclobutanetetracarboxylic acid is up to 80% under the condition as the proportion of tetramethyl cyclobutane tetracarboxylate to hydrochloric acid 1∶ 3,the reaction time 20 h and the reaction temperature 80 ℃;the yield of cyclobutanetetracarboxylic dianhydride is up to 84.0% under the condition as the proportion of cyclobutanetetracarboxylic acid to acetic anhydride 1∶ 6,the reaction time 25 h and the reaction temperature 140 ℃.