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Visible light catalyzed cross-coupling hydrogen desorption method

A cross-coupling, visible light technology, used in organic chemistry methods, chemical instruments and methods, physical/chemical process catalysts, etc.

Active Publication Date: 2013-12-18
TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But until now, there have been no patents or literature reports on visible light-catalyzed cross-coupling dehydrogenation reactions, that is, visible light-catalyzed cross-coupling reactions between tertiary amines and nucleophiles in an inert gas atmosphere without any oxidant, accompanied by hydrogen evolution

Method used

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  • Visible light catalyzed cross-coupling hydrogen desorption method
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  • Visible light catalyzed cross-coupling hydrogen desorption method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Synthesis of Graphene Oxide

[0047] (1) Expansion treatment of graphite

[0048] Heat 9mL of concentrated sulfuric acid to 80°C, add 1.6g of potassium peroxodisulfate and 1.6g of phosphorus pentoxide, stir at this temperature to completely dissolve the solid, then slowly add 2g of 320 mesh flake graphite, and finish adding within 5min , the mixture was reacted at 80°C for 4.5h, after the reaction was completed and cooled to room temperature, 350mL of deionized water was added, and after standing for 12h, the mixture was filtered through a 0.2μm filter membrane, and the residual acid and solids were washed with a large amount of water. Place at room temperature for 12h.

[0049] (2) Oxidation of expanded graphite

[0050] Take 80mL of concentrated sulfuric acid and place it in an ice bath at 0°C, add the expanded graphite obtained in step (1) into the sulfuric acid solution, then slowly add 10g of potassium permanganate under stirring, and ensure that the temperature ...

Embodiment 2

[0054] Synthesis of water-soluble graphene modified with sulfonic acid groups

[0055] Take 40mL of the graphene oxide solution obtained in 1, and use 5wt% Na 2 CO 3 Adjust the pH to 9-10. Add 160mg of sodium borohydride, react at 80°C for 1h, centrifuge after the reaction, wash the solid with water twice, then disperse in water to make a 0.5mg / mL dispersion, then add diazonium hydrochloride containing 0.095M p-sulfonic acid benzene 3.6 mL of salt, reacted in an ice bath for 2 hours, after the reaction was completed, 150 mL of acetone was added to the solution to precipitate a precipitate, which was centrifuged and washed three times with an acetone / water mixed solvent with a volume ratio of 3:1 to obtain The solid was dried in an oven at 50° C. and redispersed (ultrasonic power 150 W) into a 0.5 mg / mL aqueous solution.

Embodiment 3

[0057] Synthesis of water-soluble graphene-supported ruthenium dioxide nanoparticles modified with sulfonic acid groups

[0058] (1) Mix 30mL, 0.5mg / mL sulfonic acid-modified graphene aqueous solution with 80mL deionized water, stir, and then use ultrasonic treatment until clear (ultrasonic power is 150W) to obtain a uniform dispersion;

[0059] (2) Add 10mL, 0.0085mmol / L aqueous solution of ruthenium trichloride to the dispersion liquid, stir, and then obtain a uniform dispersion liquid through ultrasonic treatment (ultrasonic power is 150W);

[0060] (3) Add 10 mL, 0.082 mmol / L aqueous solution of trisodium citrate dihydrate to the dispersion liquid, and stir;

[0061] (4) Pass argon gas through the dispersion to remove oxygen, heat the dispersion system in an argon atmosphere, the temperature is controlled at 95°C, and the time is 10h;

[0062] (5) Centrifuge the reacted aqueous solution, wash 5 times with deionized water, centrifuge again, and finally wash with methanol, ...

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Abstract

The invention discloses a visible light catalyzed cross-coupling hydrogen desorption method. The method takes an organic dye as the photo-sensitizer, adopts platinum sol, palladium sol, hydrated ruthenium dioxide, hydrated ruthenium trioxide, ruthenium sulphate, ruthenium nitrate, or hydrated ruthenium dioxide nano particles loaded on water-soluble graphene as the catalyst, utilizes visible lights to irradiate a solution of tertiary amine and nucleophilic reagent in an atmosphere of inert gas without any oxidant, and only obtains cross-couple products and hydrogen gas. The method has the advantages of high reaction efficiency, atom economy, and environment-friendliness, and develops a novel reaction type.

Description

technical field [0001] The invention belongs to the technical field of catalytic synthesis, relates to a method for cross-coupling dehydrogenation, in particular to a method for visible-light catalyzed cross-coupling dehydrogenation of tertiary amines and nucleophiles. Background technique [0002] With the continuous development of society and economy, human society is becoming more and more aware of the enrichment and contribution of chemistry to the material world such as energy, materials, medicines, and food; Through waste water, waste gas, waste residue, etc., it is discharged to the earth on which we live. The increasingly severe environmental pollution and energy crisis have prompted people to develop energy-economical reactions, that is, chemical reactions must meet the requirements of green chemistry and minimize the energy consumption required for reactions. The biggest feature of green chemistry is that scientific methods of pollution prevention are adopted at t...

Claims

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Application Information

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IPC IPC(8): C07B37/00C07D401/04C07D217/14C07F9/62B01J23/46
Inventor 吴骊珠孟庆元钟建基
Owner TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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