Preparation method of 2, 5-bis (benzoxazole-2-) furan

A technology of benzoxazole and furan, applied in the field of preparation of 2,5-bisfuran

Pending Publication Date: 2022-06-07
黄石市利福达医药化工有限公司 +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But there is no good method for the industrialized production of 2,5-bis(benzoxazole-2-)furan at present

Method used

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  • Preparation method of 2, 5-bis (benzoxazole-2-) furan
  • Preparation method of 2, 5-bis (benzoxazole-2-) furan
  • Preparation method of 2, 5-bis (benzoxazole-2-) furan

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preparation example Construction

[0009] The invention provides a preparation method of 2,5-bis(benzoxazole-2-)furan, which is characterized in that the method comprises: making furan-2,5-dicarboxylic acid and o-aminophenol in a solvent A condensation reaction occurs under the action of a catalyst, the solvent is: 1-methylnaphthalene, and the catalyst is boric acid;

[0010] The chemical reaction principle is:

[0011]

[0012] Wherein, in the present invention, the amount of furan-2,5-dicarboxylic acid and o-aminophenol is not particularly limited, as long as condensation reaction can occur, but from the perspective of more efficient reaction, the furan-2,5 - The molar ratio of dicarboxylic acid and said o-aminophenol is preferably 1:(2-2.2).

[0013] The present invention also has no particular limitation on the amount of the solvent and the catalyst. The amount of the solvent may be 9-10 times the mass of the furan-2,5-dicarboxylic acid, and the amount of the catalyst may be the 0.15-0.2 times the mass...

Embodiment 1

[0024] Add 1200L of 1-methylnaphthalene, 124.8kg of furan-2,5-dicarboxylic acid, and 174.4kg of o-aminophenol into the cleaned 2000L stainless steel reactor (with nitrogen pipe, condenser, thermometer, water separator, etc.) , Boric acid 20kg. At this time, the molar ratio of furan-2,5-dicarboxylic acid and o-aminophenol was 1:2, the amount of 1-methylnaphthalene was 9.6 times the mass of furan-2,5-dicarboxylic acid, and the amount of boric acid was It is 0.16 times the mass of furan-2,5-dicarboxylic acid.

[0025] After feeding, nitrogen was introduced at a constant rate, kept at 3 cubic meters per hour, started stirring, slowly heated to 140 °C with heat-conducting oil, kept at 140 °C for 3 hours, then heated to 200 °C, and kept at 200 °C for 5 hours for a total of 5 hours. About 57.6 kg of water distilled during the reaction was obtained.

[0026] After the reaction is completed, the 1-methylnaphthalene solvent is distilled out under the negative pressure of the water flu...

Embodiment 2

[0032] Add 1125L of 1-methylnaphthalene, 124.8kg of furan-2,5-dicarboxylic acid, 176kg of o-aminophenol, Boric acid 25kg. At this time, the molar ratio of furan-2,5-dicarboxylic acid and o-aminophenol was 1:2.02, the amount of 1-methylnaphthalene was 9 times the mass of furan-2,5-dicarboxylic acid, and the amount of boric acid was It is 0.2 times the mass of furan-2,5-dicarboxylic acid.

[0033] After feeding, nitrogen was introduced at a constant rate, kept at 2 cubic meters per hour, started stirring, slowly heated to 150°C with heat-conducting oil, kept at 150°C for 2 hours, and then heated to 210°C, kept at 210°C for 4 hours, for a total of 4 hours. About 57.6 kg of water distilled during the reaction was obtained.

[0034] After the reaction is completed, the 1-methylnaphthalene solvent is distilled out under the negative pressure of the water flushing pump until there is no distillation, and the steamed 1-methylnaphthalene is reused for the next batch of reactions. Co...

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Abstract

The present invention provides a 2, 5-bis (benzoxazole-2-) furan preparation method, which is characterized in that furan-2, 5-dicarboxylic acid and ortho-aminophenol are subjected to a condensation reaction in a solvent under the action of a catalyst, the solvent is 1-methylnaphthalene, and the catalyst is boric acid. When the method provided by the invention is used for producing the 2, 5-bis (benzoxazole-2-) furan, the yield of the 2, 5-bis (benzoxazole-2-) furan can reach 95% or above, and industrial mass production can be realized. Therefore, the method provided by the invention can meet the large demand of the market on the 2, 5-bis (benzoxazole-2-) furan serving as a degradable fluorescent whitening agent.

Description

technical field [0001] The present invention relates to a preparation method of 2,5-bis(benzoxazole-2-)furan. Background technique [0002] At present, the fluorescent whitening agents used in the market are all non-degradable fluorescent whitening agents, which will cause residues to the environment. With the increasing environmental protection requirements, there is an increasing demand for degradable fluorescent whitening agent products. . [0003] 2,5-Bis(benzoxazole-2-)furan is known to whiten acrylic fibers (polyacrylonitrile fibers) and their blends. But there is no good method for the industrial production of 2,5-bis(benzoxazole-2-)furan. SUMMARY OF THE INVENTION [0004] Based on the above situation, the present invention has developed a preparation method of 2,5-bis(benzoxazole-2-)furan as a degradable bio-based fluorescent whitening agent. - High yield of bis(benzoxazole-2-)furan. [0005] The invention provides a preparation method of a degradable bio-based...

Claims

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Application Information

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IPC IPC(8): C07D413/14
CPCC07D413/14
Inventor 成家钢王成
Owner 黄石市利福达医药化工有限公司
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