Method for preparing phosphine guanidine compound

A technology for compounds and rare earth complexes, applied in the application field of metal organic complexes, can solve the problems of difficult synthesis of catalyst structures, difficult to realize industrial production, and unsatisfactory yields, and achieve simple and controllable reaction processes. Short time, high productivity

Active Publication Date: 2019-10-22
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Either the reaction temperature is relatively high, or the amount of catalyst used is relatively large, some catalysts have complex structures and are difficult to synthesize, and some yields cannot meet the requirements, making it difficult to realize industrial production

Method used

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  • Method for preparing phosphine guanidine compound
  • Method for preparing phosphine guanidine compound
  • Method for preparing phosphine guanidine compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Embodiment one: Yb[N(SiMe 3 ) 2 ] 2 Catalytic Synthesis of Phosphineguanidine from Diphenylphosphine and N,N'-Diisopropylcarbodiimide

[0025] Under an inert gas atmosphere, add diphenylphosphine (93.1mg, 0.5mmol) to the reaction flask after dehydration and deoxygenation treatment, and then add Yb[N(SiMe 3 ) 2 ] 2 Toluene solution (0.025 mL, 0.0025 mmol), then add N,N'-diisopropylcarbodiimide (63.1mg, 0.5mmol) with a pipette gun, react at room temperature for 1h, add CDCl 3 Dubbed into a solution. Calculated 31 The P spectrum yield was 95%. The solution was dried under reduced pressure, extracted and filtered with n-hexane to obtain a colorless transparent solution, and then the solvent was dried under reduced pressure, and the reactant was recrystallized in hexane to obtain the corresponding phosphine guanidine. i PrN=C(PPh 2 )(NH i Pr).

Embodiment 2

[0026] Embodiment two: Eu[N(SiMe 3 ) 2 ] 2 Catalytic Synthesis of Phosphineguanidine from Diphenylphosphine and N,N'-Diisopropylcarbodiimide

[0027] Under an inert gas atmosphere, add diphenylphosphine (93.1mg, 0.5mmol) to the reaction flask after dehydration and deoxygenation treatment, and then add Eu[N(SiMe 3 ) 2 ] 2 Toluene solution (0.025 mL, 0.0025 mmol), then add N,N'-diisopropylcarbodiimide (63.1mg, 0.5mmol) with a pipette gun, react at room temperature for 1h, add CDCl 3 Dubbed into a solution. Calculated 31 The P spectrum yield was 90%. The solution was dried under reduced pressure, extracted and filtered with n-hexane to obtain a colorless transparent solution, and then the solvent was dried under reduced pressure, and the reactant was recrystallized in hexane to obtain the corresponding phosphine guanidine. i PrN=C(PPh 2 )(NH i Pr).

Embodiment 3

[0028] Embodiment three: Sm[N(SiMe 3 ) 2 ] 2 Catalytic Synthesis of Phosphineguanidine from Diphenylphosphine and N,N'-Diisopropylcarbodiimide

[0029] Under an inert gas atmosphere, add diphenylphosphine (93.1 mg, 0.5 mmol) to the reaction flask after dehydration and deoxygenation treatment, and then add Sm[N(SiMe 3 ) 2 ] 2 Toluene solution (0.025 mL, 0.0025 mmol), then add N,N'-diisopropylcarbodiimide (63.1mg, 0.5mmol) with a pipette gun, react at room temperature for 1h, add CDCl 3 Dubbed into a solution. Calculated 31 The P spectrum yield was 92%. The solution was dried under reduced pressure, extracted and filtered with n-hexane to obtain a colorless transparent solution, and then the solvent was dried under reduced pressure, and the reactant was recrystallized in hexane to obtain the corresponding phosphine guanidine. i PrN=C(PPh 2 )(NH i Pr).

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Abstract

The invention relates to a method for preparing a phosphine guanidine compound. The method comprises steps as follows: under water-free and oxygen-free conditions and under nitrogen protection, diphenylphosphine, a disilylamine rare earth complex and carbodiimide are mixed uniformly in sequence to react to obtain the phosphine guanidine compound. The disilylamine rare earth complex is obtained bycatalyzing a phosphine hydrogenation reaction of carbodiimide and diphenylphosphine in a high-activity manner under the mild condition (room temperature), and the dosage of a catalyst is only 0.1%-0.5% of the molar weight of carbodiimide; the reaction speed is very high, and the yield of 95% or above can be obtained after 60 min of reaction; Compared with existing catalysis systems, the dosage ofthe catalyst is reduced, the yield is increased, short time is required, the reaction conditions are mild, and atom economy synthesis is highly met.

Description

[0001] The present invention belongs to the application of disilamine rare earth complexes in catalyzing the phosphine hydrogenation reaction of carbodiimide and diphenylphosphine. The application date is December 4, 2017, and the application number is 201711263115X. Application, which belongs to the part of product preparation method. technical field [0002] The invention relates to an application technology of a metal organic complex, in particular to the application of a disilamine rare earth complex in catalyzing the phosphine hydrogenation reaction of carbodiimide and diphenylphosphine. Background technique [0003] Phosphineguanidines are a class of organic compounds containing heteroatoms. Phosphineguanidine compounds have a wide range of applications, not only as building blocks in organic synthesis, but also as ligands for various metals. At the same time, the research on flame retardants is gradually deepening. [0004] The easiest way to synthesize phosphineguan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22C07F9/50
CPCC07F9/5036B01J31/1805B01J2531/37Y02P20/584
Inventor 薛明强武振杰顾佳丽朱章野郑煜沈琪
Owner SUZHOU UNIV
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