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Method for preparing cyclic ether through dehydration cyclization of diol

A technology of dehydration cyclization and cyclic ether, which is applied in the field of catalysis, can solve problems such as research and technology that have not been reported, and achieve the effects of no metal participation, high product yield, and strong industrial application value

Pending Publication Date: 2022-05-06
INST OF CHEM CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The research and technology of preparing cyclic ethers from diols catalyzed by ionic liquids under metal-free conditions have not been reported

Method used

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  • Method for preparing cyclic ether through dehydration cyclization of diol
  • Method for preparing cyclic ether through dehydration cyclization of diol
  • Method for preparing cyclic ether through dehydration cyclization of diol

Examples

Experimental program
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Effect test

Embodiment 1

[0057] Embodiment 1, ionic liquid [SO 3 H-BMIm][OTf] Catalyzed Dehydration of 1,4-Butanediol to Tetrahydrofuran

[0058] Put 0.05 moles of ionic liquid and 0.2 moles of 1,4-butanediol in a 20 ml temperature-resistant glass reaction tube, seal it; move it to an oil bath at 120°C, stir and heat for 12 hours for dehydration and cyclization reaction; immerse the reaction tube in The reaction was terminated in ice water, and then it was placed at room temperature for a period of time; then, the phase composition of tetrahydrofuran was analyzed by gas chromatography, and the phase composition of ionic liquid was analyzed by nuclear magnetic resonance. According to the analysis results, the conversion rate of 1,4-butanediol is 100%, the selectivity of THF is 100%, and the yield is >99%.

Embodiment 2

[0059] Example 2, ionic liquid [HO-BMIm][OTf] catalyzed dehydration of 1,4-butanediol to prepare tetrahydrofuran

[0060] Put 0.05 moles of ionic liquid and 0.2 moles of 1,4-butanediol in a 20 ml temperature-resistant glass reaction tube, seal it; move it to an oil bath at 120°C, stir and heat for 12 hours for dehydration and cyclization reaction; immerse the reaction tube in The reaction was terminated in ice water, and then it was placed at room temperature for a period of time; then, the phase composition of tetrahydrofuran was analyzed by gas chromatography, and the phase composition of ionic liquid was analyzed by nuclear magnetic resonance. According to the analysis results, the conversion rate of 1,4-butanediol is 100%, the selectivity of THF is 100%, and the yield is >99%.

Embodiment 3

[0061] Embodiment 3, ionic liquid [SO 3 H-PrMIm][OTf] Catalyzed Dehydration of 1,4-Butanediol to Tetrahydrofuran

[0062] Put 0.05 moles of ionic liquid and 0.2 moles of 1,4-butanediol in a 20 ml temperature-resistant glass reaction tube, seal it; move it to an oil bath at 120°C, stir and heat for 12 hours for dehydration and cyclization reaction; immerse the reaction tube in The reaction was terminated in ice water, and then it was placed at room temperature for a period of time; then, the phase composition of tetrahydrofuran was analyzed by gas chromatography, and the phase composition of ionic liquid was analyzed by nuclear magnetic resonance. According to the analysis results, the conversion rate of 1,4-butanediol is 100%, the selectivity of THF is 100%, and the yield is >99%.

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Abstract

The invention discloses a method for preparing cyclic ether through diol dehydration cyclization. The method comprises the following steps: carrying out a diol dehydration reaction in a temperature range of 50-200 DEG C by using an ionic liquid as a solvent and a catalyst to prepare cyclic ether. The ionic liquid catalytic system provided by the invention has the advantages of high efficiency, simplicity, mildness (120 DEG C), no metal participation and the like, can efficiently catalyze glycol dehydration to prepare cyclic ether, and has a relatively high industrial application value.

Description

technical field [0001] The invention belongs to the field of catalysis, and in particular relates to a method for preparing cyclic ethers through dehydration and cyclization of diols. Background technique [0002] Cyclic ethers such as tetrahydrofuran and tetrahydropyran are important raw materials for organic synthesis and solvents with excellent performance, and are widely used in the chemical industry. Industrially, the preparation of cyclic ethers by intramolecular dehydration and cyclization of diols is a common method for the production of such substances, usually using liquid acid catalysts. This technology is mature, the process is relatively simple, and the reaction temperature is low, but there are problems such as easy corrosion of equipment, pollution of the environment, and difficulty in separation. Therefore, it is of great significance to develop new catalytic systems that are clean, pollution-free, and non-corrosive. [0003] Ionic liquids are composed of o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/08C07D307/06C07D313/04C07D307/10C07D307/93C07D307/79
CPCC07D307/08C07D307/06C07D313/04C07D307/10C07D307/93C07D307/79
Inventor 刘志敏王欢赵燕飞韩布兴
Owner INST OF CHEM CHINESE ACAD OF SCI
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