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Organic phosphorus ligand as well as preparation method and application thereof

A phosphine ligand, an independent technology, applied in the field of organophosphorus ligand and its preparation, can solve the problems of long process route, corrosive reaction system, harsh reaction conditions, etc.

Pending Publication Date: 2021-12-31
SOUTH UNIVERSITY OF SCIENCE AND TECHNOLOGY OF CHINA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the indirect process has been industrialized, it has the disadvantages of high corrosion to equipment, long process route, reduced efficiency, and high cost.
Compared with the above processes, the combination of syngas and methanol to produce ethanol has the advantages of high ethanol selectivity and fewer intermediate steps, so it has been sought after by more researchers; however, there are still reactions in most homogeneous or heterogeneous catalysis studies. Harsh conditions, high pressure (19MPa, 190Bar), high reaction temperature (190 degrees), and corrosive reaction system restrict the industrial application of this process

Method used

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  • Organic phosphorus ligand as well as preparation method and application thereof
  • Organic phosphorus ligand as well as preparation method and application thereof
  • Organic phosphorus ligand as well as preparation method and application thereof

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preparation example Construction

[0024] Aiming at the deficiencies of the prior art, the present invention provides a novel phosphine ligand and its preparation method. The mixture of synthesis gas and methanol can obtain fuel in one pot under the condition of mixing the phosphine ligand and the Rh / Ru bimetallic catalyst precursor. Ethanol, through process optimization, the reaction can be carried out under mild conditions, and the selectivity is high, which can greatly reduce the cost, and has a good industrialization prospect, huge economic benefits and social value.

[0025] In view of the deficiencies in the prior art, the object of the present invention is to provide a novel phosphine ligand, which has a chemical structure as shown in the following formula (I) or formula (II),

[0026]

[0027] in,

[0028] x 1 、X 2 , Y 1 , Y 2 each independently N or CR 6 ;

[0029] R 1 , R 2 , R 6 independently H, F, Cl, Br, I, cyano, trifluoromethyl, alkyl, alkenyl, alkoxy, alkylmercapto, dialkylamino, ami...

Embodiment 1

[0088] The general preparation method is as follows

[0089]

[0090] At room temperature, add 10 to 12.5 mmol of bisarylphosphine hydrogen 2 into a 250 ml three-necked flask, vacuumize and fill with argon, repeat the process 3 times, add 30 mL of dry THF (tetrahydrofuran) as a solvent in an argon atmosphere, and then The three-necked flask was placed in an ice bath, and 15 mmol of n-butyllithium (1.6M n-hexane solution) was slowly added dropwise. The reaction solution changed from clear to dark red solution, indicating that P-Li had been generated, and the addition was completed. After that, make it return to room temperature naturally and continue to stir for 2 hours; then, under room temperature, add gem-dialkyl-1,3-diX propane 1 (5mmol) dropwise in THF solution, monitor until after the reaction ends, use Quench the reaction with degassed saturated ammonium chloride aqueous solution, extract with dichloromethane, dry over anhydrous sodium sulfate, remove volatile reagent...

Embodiment 2

[0096]

[0097] Under room temperature conditions, weigh 1.0 times the equivalent of 1,8-dibromonaphthalene in a 250 ml three-necked flask, vacuumize and fill with argon, repeat 3 times, add 150 mL of dry Et in an inert gas O (diethyl ether) as a solvent, and then The three-necked reaction flask was placed in an ice bath, and 2.2 times of equivalent n-butyl lithium (1.6M in n-hexane) was slowly added dropwise. After the dropwise addition, it was naturally returned to room temperature and continued to stir for 2 hours; subsequently, in Under ice-bath conditions, 2.2 times the equivalent of diphenylphosphine chloride solution was added dropwise. After the reaction was completed, the reaction was quenched with degassed saturated ammonium chloride aqueous solution, extracted with dichloromethane, dried over anhydrous sodium sulfate, and decompressed. The volatile reagents were removed under certain conditions, and finally, a short chromatographic separation was carried out quick...

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Abstract

The invention provides a novel phosphine ligand and a preparation method thereof. Fuel ethanol can be obtained from a mixture of synthetic gas and methanol through a one-pot method under the condition that a phosphine ligand and an Rh / Ru bimetallic catalyst precursor are mixed. Through process optimization, the reaction can be carried out under mild conditions, the selectivity is high, and the cost can be greatly reduced. The novel phosphine ligand has good industrialization prospects and huge economic benefits and social values.

Description

technical field [0001] The invention relates to the field of organic chemistry, organophosphorus ligand and its preparation method and application. Background technique [0002] Organophosphine ligands play a very important role in fine chemical fields such as organic synthesis, medicine, materials, and pesticides. Therefore, organophosphorus chemists have continued to devote themselves to this research field through continuous efforts. In 1980, since the Hirao group reported the first case of palladium-catalyzed direct cross-coupling of [P]H compounds with organohalides to construct PC bonds, The reaction conditions are mild and the substrates are applicable to a wide range, which opens the first transition metal-catalyzed cross-coupling reaction of [P]H compounds, and has been widely developed and applied. The current synthesis of p-arylphosphine ligands has made great progress. But it is worth mentioning that the Hirao-type coupling reaction is mainly limited to the syn...

Claims

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Application Information

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IPC IPC(8): C07F9/50B01J31/24B01J31/22B01J31/20C07C29/32C07C31/08
CPCC07F9/5022C07F9/5031B01J31/2409B01J31/2213B01J31/20C07C29/32B01J2531/821B01J2531/822B01J2531/0219B01J2231/4205C07C31/08Y02P20/52
Inventor 张继树温佳琳张绪穆
Owner SOUTH UNIVERSITY OF SCIENCE AND TECHNOLOGY OF CHINA
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