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3,4-ethylenedioxythiophene preparation method

A technology of ethylenedioxythiophene and a manufacturing method, which is applied in the field of improvement 3, can solve the problems of limited yield improvement effect, unsuitability for mass production, and high solvent residue, and achieves an environmentally friendly preparation process, high yield, and fast reaction rate. Effect

Inactive Publication Date: 2013-02-13
FAR EASTERN NEW CENTURY COPRRATION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this preparation process has problems such as too high residual solvent and the toxicity of the solvent, which is not suitable for mass production, and the effect of improving the yield is still limited.

Method used

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  • 3,4-ethylenedioxythiophene preparation method
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  • 3,4-ethylenedioxythiophene preparation method

Examples

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preparation example Construction

[0012] In order to achieve the above object, the preparation method according to the present invention comprises the following steps:

[0013] Provide monothiodiacetic acid, mix it with ethanol, and add sulfuric acid as a catalyst, in a microwave reactor with a frequency of 2.45GHz, with a power of 500-1000W, carry out the esterification reaction for 15-30 minutes, To obtain diethyl thiodiacetate, as shown in the following formula (A).

[0014]

[0015] According to the microwave reactor of the present invention, the reaction is carried out inside the cavity by adjusting different powers. It is well known in the art that the use of microwave reactor heating to replace traditional heating (for example: water bath heating, alcohol lamp heating, heating pack heating, etc.) has been widely disclosed in the field of organic synthesis. The microwave heating reaction is to use the polar molecules in the reaction solution to vibrate under the effect of electromagnetic waves in an ...

Embodiment A1

[0064] Get 15.015 grams of thiodiacetic acid (2,2'-thiodiacetic acid, Acros, Belgium), 55.284 grams of ethanol (ECHO, Taiwan), and 4.9 grams of sulfuric acid (Sigma-Aldrich, Switzerland), add to 20 grams of toluene (ECHO, Taiwan), after mixing and stirring until completely dissolved, move to a microwave reactor, adjust the frequency to 2.45 GHz, set the microwave power to 500 watts, and the reaction time is 30 minutes.

[0065] A Dean-Stark water removal device was set up outside the microwave reactor to remove water, and the solution temperature during the heating process was about 86-87°C and refluxed. After the reaction, the temperature was lowered, and the pH was titrated to 7-7.5 with NaOH aqueous solution to terminate the reaction. It was extracted three times with ethyl acetate / n-hexane (9 / 1) and saturated brine, and the organic layer was taken out, dried over anhydrous magnesium sulfate, and filtered. The solvent was removed by rotary concentration and then dried unde...

Embodiment A2

[0067] The implementation is as described in Example A1, but the microwave power is set to 750 watts, and the reaction time is 20 minutes. A yield of 92.7% was obtained.

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Abstract

A 3,4-ethylenedioxythiophene preparation method is characterized in that 3,4-ethylenedioxythiophene is synthesized through utilizing microwave heating, so the 3,4-ethylenedioxythiophene preparation yield is greatly improved, the whole reaction time is reduced, the energy loss in the heating period is reduced, the solvent application amount is reduced, and the harm to the environment is reduced.

Description

technical field [0001] The present invention relates to a method for preparing 3,4-ethylenedioxythiophene, in particular to a method for increasing the yield of 3,4-ethylenedioxythiophene by using a microwave method instead of a traditional heating method. Background technique [0002] It is well known in the art that 3,4-ethylenedioxythiophene (3,4-ethylenedioxythiophene, EDOT) is a monomer used to prepare polyethylenedioxythiophene (PEDOT). Because polyethylenedioxythiophene has high conductivity, high transparency, good heat resistance, good hydrolysis resistance and easy processing, it is often used to prepare organic light-emitting diodes (OLEDs), solar cells, organic thin-film transistors (OTFT ), supercapacitors, flexible electronic paper and other devices, the electron transport layer is widely used in the field of optoelectronics. [0003] Many scholars have studied and discussed about the synthetic method of 3,4-ethylenedioxythiophene. However, the method for synt...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D495/04
Inventor 梁乃云蔡惠珊柯青炜曾智远
Owner FAR EASTERN NEW CENTURY COPRRATION