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Preparation method of heteronuclear metal complexes and cyclic carbonates catalyzed by them

A technology for metal complexes and compounds is applied in the field of preparation of cyclic carbonates, which can solve the problems of catalyst dosage and reaction pressure reduction, and achieve the effects of simple post-treatment, good reaction selectivity and high yield.

Active Publication Date: 2021-06-22
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the catalyst dosage and reaction pressure of this reaction need to be further reduced

Method used

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  • Preparation method of heteronuclear metal complexes and cyclic carbonates catalyzed by them
  • Preparation method of heteronuclear metal complexes and cyclic carbonates catalyzed by them
  • Preparation method of heteronuclear metal complexes and cyclic carbonates catalyzed by them

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Diethylene glycol amine bridged bisaryloxyyttrium-benzyloxymagnesium complex L 2 Y 2 Mg(OCH 2 Ph) 2 (THF) 2 Synthesis:

[0051] The reaction scheme is as follows (RE is yttrium):

[0052]

[0053] (1) Put 1.63 grams of H 3 L (3.0 mmol) was dissolved in tetrahydrofuran and added to a solution containing 1.31 g of YCp 3 (THF) (3.0 mmol) in tetrahydrofuran solution, the reaction was stirred at 25°C for 24 hours, and the system was a pale yellow transparent solution.

[0054] (2) 1.5 mL of a hexane solution of tetrabutylmagnesium (1.5 mmol, 1.0 mol / L) was added to 3.0 mL of a tetrahydrofuran solution (3.0 mmol, 1.0 mol / L) of benzyl alcohol (ie, benzyl alcohol) while stirring. liter), then 10 mL of tetrahydrofuran was added to dilute the reaction solution, and the reaction was carried out at 25° C. overnight. The system was a colorless and transparent solution.

[0055] (3) Mix the reaction solutions of step (1) and step (2), rinse the reaction flask with tetrahyd...

Embodiment 2

[0061] Diethylene glycol amine bridged bisaryloxyytterbium-benzyloxymagnesium complex L 2 Yb 2 Mg(OCH 2 Ph) 2 (THF) 2 Synthesis:

[0062] (1) Put 1.63 grams of H 3 L (3.0 mmol) was dissolved in tetrahydrofuran and added to a mixture containing 1.32 g of YbCp 3 (THF) (3.0 mmol) in tetrahydrofuran solution, the reaction was stirred at 25° C. for 24 hours, and the system was a bright yellow transparent solution.

[0063] (2) 1.5 mL of a solution of tetrabutylmagnesium in hexane (1.5 mmol, 1.0 mol / L) was added to 3.0 mL of a solution of benzyl alcohol in tetrahydrofuran (3.0 mmol, 1.0 mol / L) with stirring, Then 10 mL of tetrahydrofuran was added to dilute the reaction solution, and the reaction was carried out at 25° C. overnight. The system was a colorless and transparent solution.

[0064] (3) Mix the reaction solutions of step (1) and step (2), rinse the reaction flask with tetrahydrofuran, and react in an oil bath at 50° C. for 3 days.

[0065] (4) The solvent was remo...

Embodiment 3

[0068] Diethylene glycol amine bridged bisaryloxyneodymium-benzyloxymagnesium complex L 2 Nd 2 Mg(OCH 2 Ph) 2 (THF) 2 Synthesis:

[0069] (1) Put 1.63 grams of H 3 L (3.0 mmol) was dissolved in tetrahydrofuran and added to a solution containing 1.23 g of NdCp 3 (THF) (3.0 mmol) in tetrahydrofuran solution, the reaction was stirred at 25° C. for 24 hours, and the system was a blue transparent solution.

[0070] (2) 1.5 mL of a solution of tetrabutylmagnesium in hexane (1.5 mmol, 1.0 mol / L) was added to 3.0 mL of a solution of benzyl alcohol in tetrahydrofuran (3.0 mmol, 1.0 mol / L) with stirring, Then 10 mL of tetrahydrofuran was added to dilute the reaction solution, and the reaction was carried out at 25° C. overnight. The system was a colorless and transparent solution.

[0071] (3) Mix the reaction solutions of step (1) and step (2), rinse the reaction flask with tetrahydrofuran, and react in an oil bath at 50° C. for 3 days.

[0072] (4) The solvent was removed unde...

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Abstract

The invention discloses a method for preparing cyclocarbonate by converting carbon dioxide and epoxy compounds under the action of a catalyst, and belongs to the technical field of organic compound preparation. The catalyst of the method of the present invention is easy to prepare, the yield is high, the reaction conditions are mild, the highly selective conversion of carbon dioxide and alkylene oxide compounds can be realized under ambient temperature and normal pressure, thereby synthesizing cyclocarbonate compounds, and the substrate is universal wide. The technical scheme of the present invention is as follows: a cyclocarbonate is synthesized by using a diethylene glycol amino bridged bisaryloxy rare earth-benzyloxy magnesium heteronuclear metal complex and a quaternary ammonium salt as a catalyst system, and carbon dioxide and an alkylene oxide compound as reactants compound.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a preparation method of a heteronuclear metal complex and a catalyzed cyclic carbonate. Background technique [0002] carbon dioxide (CO 2 ) as an ideal C1 resource widely exists in nature and industrial waste gas, and the effective use of carbon dioxide can not only promote economic development but also contribute to environmental protection. of which CO 2 The atom utilization rate of reacting with alkylene oxide to generate cyclic carbonate is as high as 100%, and the existence of cyclic carbonate can directly promote the development of various industries. Therefore, many scientists have been working on the development of this reaction for more than a century, especially in the past 20 years. [0003] Since 2010, North's research group has found that with the same amount of catalyst and the same amount of catalyst at 25 °C and 1 atmosphere for 24 hours, the binuclear Al-sale...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F19/00B01J31/22C07D317/46C07D317/36C07D317/44C07D493/04
Inventor 姚英明华琳琰
Owner SUZHOU UNIV