Preparation method of 3,4-ethylene dioxy thiophene
A technology of ethylenedioxythiophene and hydroxysodium thiophene, which is applied in the direction of organic chemistry, can solve the problems of increased cost, labor and energy consumption, impact of EDOT quality, difficult purification to high-purity grade and other problems in industrialization, so that the reaction conditions are not harsh and the products High and stable yield, simple and easy operation
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[0019] The present invention will be further described below in conjunction with the examples, but not limited thereto.
[0020] A kind of preparation method of 3,4-ethylenedioxythiophene, comprises the following steps:
[0021] (1) Sulfurization reaction: under the protection of nitrogen, put 80g sodium sulfide, 500ml absolute ethanol, and 0.5g crown ether in a flask, add 122.5g (1mol) ethyl chloroacetate dropwise at room temperature, and raise the temperature to 50 ℃, keep warm for 1h, sample GC tracking, ethyl chloroacetate content ≤ 2%, the reaction is complete; filter, filter the cake with 30ml of absolute ethanol twice to wash the combined filtrate to obtain 705g, GC content 27.1%, equivalent to thiodiglycolic acid The ester was 191.4g, and the molar yield was 92.9%.
[0022] (2) Condensation, etherification and saponification, under the protection of nitrogen, add the thiodiglycolic acid ester obtained above into the flask, control the temperature at 40-50°C, add 150g ...
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