Z. Wen-jun
2008
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Journal
Henan Chemical Industry
Abstract
3,4-Ethylenedioxythiophene(EDOT) is synthesized using thiodiglycolic acid as starting material via five reactions.Firstly,thiodiglycolic acid reactes with methanol to synthesize thiodiglycolic acid dimethyl ester by esterify reaction with strong sulfuric acid catalyzer,the yield is 93.2%;product reactes with diethyl oxalate to synthesize 3,4-dihydrothieno-2,5-dicarboxylic acid dimethyl ester by Claisen condensation reaction,the yield is 92.0%,then 3,4-dihydrothieno-2,5-dicarboxylic acid dimethyl ester via the step of O-alkylation reaction and use tetrabutyl ammonium bromide for phase transfer catalyst,to get 3,4-ethylenedioxythiophene-2,5-dicarboxylic acid dimethyl ester,which to hydrolyze to give 3,4-ethylenedioxythiophene-2,5-dicarboxylic acid;3,4-ethylenedioxythiophene-2,5-dicarboxylic acid take away two molecule of CO2 to get the final product EDOT in DMSO solvent,N2 protect and cubric carbonate catalyze.Structures of intermediate products and final products are characterized by IR spectra and determined assay by GC,the total yield is 34.6%.