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Preparation method for 3,4-dibromothiophene

A technology of dibromothiophene and tetrabromothiophene, which is applied in the direction of organic chemistry and can solve problems such as difficult product separation

Inactive Publication Date: 2014-03-05
徐广苓
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, thiophene and hydrobromic acid solutions are often used to synthesize 3,4-dibromothiophene in the presence of various catalysts. However, it is inevitable that not only various bromothiophenes exist in the product, but also the above-mentioned product is due to the melting point, Difficult to separate due to similar boiling points

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0009] Add 1 mole of 2,3,4,5-tetrabromothiophene, 2 moles of acetic acid and water into the reaction vessel, use 3 moles of zinc powder with a purity of 95% as a catalyst to react for 2 hours at room temperature, and divide the zinc powder into 5 times Add it into the reaction solution; then heat it to 55-70°C and reflux for 2-4 hours. After the reaction is completed, distill under reduced pressure and collect the fraction at 100°C to obtain 3,4-dibromothiophene. The yield of the product is 90%, and the purity is 98.74%. .

Embodiment 2

[0011] Add 1 mole of 2,3,4,5-tetrabromothiophene, 2.5 moles of acetic acid and water into the reaction vessel, use 3.5 moles of zinc powder with a purity of 95% as a catalyst to react for 2 hours at room temperature, and divide the zinc powder into 5 times Add it into the reaction solution; then heat it to 55-70°C and reflux for 2-4 hours. After the reaction is completed, distill under reduced pressure and collect the fraction at 100°C to obtain 3,4-dibromothiophene. The yield of the product is 95%, and the purity is 99.98%. .

Embodiment 3

[0013] Add 1 mole of 2,3,4,5-tetrabromothiophene, 3 moles of acetic acid and water into the reaction vessel, use 4 moles of zinc powder with a purity of 95% as a catalyst to react for 2 hours at room temperature, and divide the zinc powder into 5 times Add to the reaction solution; then heat to 55-70°C and reflux for 2-4 hours. After the reaction is completed, distill under reduced pressure and collect fractions at 100°C to obtain 3,4-dibromothiophene. The yield of the product is 91%, and the purity is 97.54%. .

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PUM

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Abstract

The invention discloses a preparation method for 3,4-dibromo thiophene. The method includes adding a raw material 2,3,4,5-tetrabromothiophene, a reductant acetic acid and a solvent water into a reaction container, reacting for 2 h at room temperature by using zinc powder as a catalyst, heating to 55-70 DEG C and reacting under refluxing for 2-4 h, performing reduced pressure distillation after the reaction is finished, and collecting the fraction at 100 DEG C, namely collecting the 3,4-dibromothiophene. The zinc powder and the acetic acid are adopted as a reduction system. The zinc powder has high activity and the reaction process can be controlled by adding the zinc powder in batches, thus saving the raw material and improving the yield and the purity of the product. The yield can reach 95% and the purity is 99.98%.

Description

technical field [0001] The invention relates to a preparation method of 3,4-dibromothiophene, which belongs to the field of fine chemicals. Background technique [0002] Since the 1980s, the synthesis and development of thiophene derivatives have been widely concerned by the academic community, especially after the formation of the new material science branch of conductive polymers, due to the widespread use of conductive polythiophene and its derivatives in the fields of modern optoelectronics and microelectronics The attractive application prospects in the fields of polythiophene and modern medicine have attracted much attention from academia and industry. Scientists have done a lot of work to clarify the relationship between substituents and the physical properties of polythiophene derivatives. The premise of synthesizing high-quality polymers is to synthesize high-purity, high-yield monomers. Due to the distribution of the microscopic electron cloud, the reactivity of t...

Claims

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Application Information

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IPC IPC(8): C07D333/28
CPCC07D333/28
Inventor 徐广苓
Owner 徐广苓
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