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Rare earth metal-organic framework material catalyst and preparation and application thereof

A rare earth metal, organic framework technology, applied in the preparation of organic compounds, organic compound/hydride/coordination complex catalysts, catalytic reactions, etc., can solve the problems of non-recyclability, low catalytic efficiency, etc., to solve the problem of poor recyclability Effect

Inactive Publication Date: 2021-06-15
SHENYANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Commonly used Lewis acids are AlCl 3 , BF 3 , TiCl 4 , SnCl 4 , but its sensitivity to water, low catalytic efficiency and non-recyclability limit its wider application

Method used

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  • Rare earth metal-organic framework material catalyst and preparation and application thereof
  • Rare earth metal-organic framework material catalyst and preparation and application thereof
  • Rare earth metal-organic framework material catalyst and preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 0.067 mmol of Tb(NO 3 ) 3 and 0.129 mmol of H 2 bct was placed into a container containing 6 ml DMF and 4 ml H 2 O in a Teflon-lined reactor and with 6 mol per liter of HNO 3 Adjust the pH of the solution to 4, stir for half an hour, put it into a reaction kettle, and place it in an oven at 170° C. for 3 days. The filter cake was obtained after suction filtration, and dried to constant weight in a dry atmosphere to obtain the active component of catalyst 1.

Embodiment 2

[0028] Example 2: Catalyzed Strecker Reaction of Aldimines

[0029] The trimethylsilyl cyanide of 0.125 millimoles, the catalyst 1 of 0.008 millimoles ([Tb 2 (HCOO) 2 (bct) 2 ]) and 0.05 mmol of aldimine were added sequentially to 0.5 ml of CDCl 3 of a standard 5mm NMR tube. Afterwards, the NMR tubes were capped and sealed with Teflon tape, and then inserted into a constant temperature water bath shaker at room temperature. This response passes 1 H-NMR spectroscopic monitoring, the conversion of the product was determined according to the ratio of the integral of the product signal to the sum of the integrals of all signals (aldimine and product).

[0030] The reaction results of catalyst 1 in Example 2 are shown in Table 1.

[0031] Table 1: Strecker reaction of aldimine with trimethylsilylcyanide catalyzed by metal catalysts

[0032]

[0033]

[0034]

[0035] a Reaction conditions: aldimine (0.05 mmol), TMSCN (0.125 mmol), catalyst3 (0.008 mmol), CDCl 3 (...

Embodiment 3

[0037] 0.067 mmol of Eu(NO 3 ) 3 and 0.129 mmol of H 2 bct was placed into a container containing 6 ml DMF and 4 ml H 2 O in a Teflon-lined reactor and with 6 mol per liter of HNO 3 Adjust the pH of the solution to 4, stir for half an hour, put it into a reaction kettle, and place it in an oven at 170° C. for 3 days. The filter cake was obtained after suction filtration, and dried to constant weight in a dry atmosphere to obtain the active component of catalyst 2.

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Abstract

The invention relates to a catalyst preparation technology, and aims to provide a rare earth metal-organic framework material catalyst as well as preparation and application thereof. The structural formula of the catalyst is [Ln2(HCOO)2(bct)2].H2O(Ln=Tb(1),Eu(2),Gd(3)), in the formula, the bct is 3,5-bis(4'-carbon-phenyl)-1,2,4-triazole. The active initiation center structure of the catalyst is a high-concentration unsaturated coordinated Lewis acid metal site on the inner surface, and the catalyst can efficiently catalyze the strecker reaction of aldimine and trimethyl silicon cyanide.

Description

technical field [0001] The invention relates to catalyst preparation technology, in particular to an invention about the preparation and application of a novel rare earth metal-organic framework material catalyst. It specifically relates to a rare earth metal whose catalytic active center is a coordination unsaturated rare earth metal site (rare earth metal includes Eu, Tb, Gd), which can catalyze a series of reactions between aldimine and trimethylsilyl cyanide (TMSCN)- Preparation technology and application of organic framework material catalyst. Background technique [0002] α-Aminonitrile is an important intermediate for the synthesis of various amino acids, and is widely used in the fields of biology and medicine. The most common and used preparation method is the Strecker reaction between aldimine and trimethylsilyl cyanide (TMSCN). Lewis acid is a commonly used catalyst for Strecker reaction, which can effectively improve the nucleophilic addition activity of trimet...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22C07C253/00C07C269/06C08G83/00C07C255/42C07C255/43C07C271/22
CPCB01J31/2239C08G83/008C07C253/00C07C269/06B01J2531/38B01J2231/322C07C255/42C07C255/43C07C271/22
Inventor 王圣燕
Owner SHENYANG UNIV
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