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Dianionic guanidine complex of rare earth and lithium and application thereof

A technology of negative ions and complexes is applied in the field of double negative ion rare earth lithium complexes to achieve the effects of reducing costs, being beneficial to purification and reducing pollution

Inactive Publication Date: 2014-12-10
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In 2003, the Richeson group in Canada reported that the structural formula is (Me 2 N)C(NiPr) 22 Ti=NC 6 f 5 Titanium (see: J.Am.Chem.Soc.125, 27, 20038101) and vanadium imides (see: F.Montilla, A.Pastor, A.Galindo, J.Organomet.Chem.2004, 689, 993-996) can be used as catalysts to successfully catalyze the addition reaction of primary aromatic amines and carbodiimides to the corresponding guanidines, but secondary amines cannot be used for this reaction
[0008] (2) The addition reaction of the existing reported aliphatic diamine and carbodiimide needs to be carried out at 100°C, and the yield is only 60%; while the addition reaction of aromatic diamine such as p-phenylenediamine and carbodiimide The reaction also needs to be carried out at a temperature of 60°C or higher, and the amount of catalyst generally needs to be 1% or even higher. Therefore, it is necessary to find a catalyst with higher activity, less dosage, and milder reaction conditions. This is not only economical, but also Convenient post-treatment of the reaction system
[0009] (3) The catalysts currently reported are basically carried out in the presence of solvents. Based on the requirements of environmental protection, a catalyst that can catalyze organic reactions without solvents is needed

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Example 1: Catalyst [{p-ClPhNLi(THF)(DME)}C(N i Pr) 2 ] 3 Synthesis of La

[0027] Weigh a certain amount of p-ClC 6 h 4 NH 2 Place in a reaction bottle that has been dehydrated and deoxygenated, add an appropriate amount of tetrahydrofuran to dissolve it, put the bottle in an ice bath, add two equivalents of n-BuLi, slowly rise to room temperature, react for 1 hour, and then place it in an ice bath , add an equivalent amount of 1,3-diisopropylcarbodiimide, slowly rise to room temperature, react for 1 hour, add a weighed LaCl 3 (pre-weighed LaCl 3 Place in a reaction flask that has been dehydrated and deoxygenated, add an appropriate amount of tetrahydrofuran, and stir to activate it under anhydrous and oxygen-free conditions for standby), after stirring at room temperature for 48 hours, remove most of the tetrahydrofuran in a vacuum, then add toluene, and heat to a slight boil , centrifuged to remove the precipitate, and the resulting solution was placed at 0°C,...

Embodiment 2

[0028] Embodiment two: Catalyst [{p-ClPhNLi(THF)(DME)}C(N i Pr) 2 ] 3 Synthesis of Nd

[0029] Weigh a certain amount of p-ClC 6 h 4 NH 2 Place in a reaction bottle that has been dehydrated and deoxygenated, add an appropriate amount of tetrahydrofuran to dissolve it, put the bottle in an ice bath, add two equivalents of n-BuLi, slowly rise to room temperature, react for 1 hour, and then place it in an ice bath , add an equivalent amount of 1,3-diisopropylcarbodiimide, slowly rise to room temperature, react for 1 hour, add weighed NdCl 3 (pre-weighed NdCl 3 Place in a reaction flask that has been dehydrated and deoxygenated, add an appropriate amount of tetrahydrofuran, and stir to activate it under anhydrous and oxygen-free conditions for standby), after stirring at room temperature for 48 hours, remove most of the tetrahydrofuran in a vacuum, then add toluene, and heat to a slight boil , centrifuged to remove the precipitate, and the resulting solution was placed at 0...

Embodiment 3

[0031] Embodiment Three: Catalyst [{p-ClPhNLi(THF)(DME)}C(N i Pr) 2 ] 3 Synthesis of Sm

[0032] Weigh a certain amount of p-ClC 6 h 4 NH 2 Place in a reaction bottle that has been dehydrated and deoxygenated, add an appropriate amount of tetrahydrofuran to dissolve it, put the bottle in an ice bath, add two equivalents of n-BuLi, slowly rise to room temperature, react for 1 hour, and then place it in an ice bath , add an equivalent amount of 1,3-diisopropylcarbodiimide, slowly rise to room temperature, react for 1 hour, add weighed SmCl 3 (pre-weighed SmCl 3 Place in a reaction flask that has been dehydrated and deoxygenated, add an appropriate amount of tetrahydrofuran, and stir to activate it under anhydrous and oxygen-free conditions for standby), after stirring at room temperature for 48 hours, remove most of the tetrahydrofuran in a vacuum, then add toluene, and heat to a slight boil , centrifuged to remove the precipitate, and the resulting solution was placed at...

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Abstract

The invention discloses a dianionic complex of rare earth and lithium, and concretely relates to a dianionic guanidine complex of rare earth and lithium with a trivalent central ion. The dianionic guanidine complex of rare earth and lithium is represented by a general formula {[ArNLi(THF)(DME)]C(NPr)2}3Ln (Ar is Ph, or p-ClPh), and in the formula, Ln which represents the central ion is a trivalent cation of a rare earth metal which is selected from one of lanthanide elements of samarium, neodymium, and lanthanum. The complex which is treated as a catalyst for a synthetic reaction for preparing biguanide from a diamine and a carbonized diamine has a highly active catalytic effect on the addition reaction of the diamine and the carbonized diamine under conditions of a temperature from room temperature to 60DEG C. The reaction has a wide substrate adaptability, and aromatic diamines and aliphatic diamines all perform high catalytic activities, so reactions can be carried out under a solvent-free condition.

Description

technical field [0001] The present invention relates to a dianion rare earth lithium complex, in particular to a dianion guanidine-based rare earth / lithium complex with a trivalent central ion and its use as a catalyst to catalyze the addition reaction of diamine and carbodiimide to prepare biguanides application. Background technique [0002] Guanidine is a class of compounds with important physiological activity, which widely exists in drugs and natural products as the main skeleton; guanidine derivatives are also widely used as an important auxiliary ligand to stabilize main group metals, transition metals, and Organometallic compounds of rare earth metals. Therefore, the study of its synthesis has important theoretical and practical value. [0003] The commonly used method for synthesizing guanidine is to use an amine and a suitable electrophilic amidine reagent or a reagent that can generate a guanidine structure to react. This method uses the amine to replace the lea...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F19/00B01J31/22C07C277/08C07C279/18C07C279/04C07D213/74C07D239/50
Inventor 沈琪张兴敏王传勇
Owner SUZHOU UNIV