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Nitrogen-oxygen-containing lithium-magnesium bimetallic catalyst and its preparation method and application

A bimetallic catalyst, ionic technology, applied in the reduction preparation of oxygen-containing functional groups, catalytic reaction, preparation of amino compounds, etc., can solve the problems of insufficient catalyst activity, long reaction time, difficult preparation, etc., and achieve high selectivity and catalytic performance. The effect of activity, simple preparation method and low condition requirements

Inactive Publication Date: 2021-03-23
鄂尔多斯应用技术学院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The purpose of the present invention is to solve the technical problems that the catalysts used in the existing MPV reaction have complex structures, are not easy to prepare, the catalyst activity is not high enough, the dosage is large, and the reaction time is long, and a nitrogen-oxygen ion-containing lithium-magnesium bimetallic catalyst and Its preparation method and application, the catalyst is easy to synthesize, the reaction conditions are mild, and it has high catalytic activity for the selective synthesis of primary and secondary alcohols

Method used

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  • Nitrogen-oxygen-containing lithium-magnesium bimetallic catalyst and its preparation method and application

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Embodiment 1

[0017] Nitrogen-containing oxygen ion type lithium-magnesium bimetallic catalyst in the present embodiment, its structural formula is:

[0018]

[0019] In the formula: three lithium atoms respectively form a four-coordination mode with the oxygen atom in the ligand, two nitrogen atoms and the oxygen atom of another ligand, and form two five-membered rings sharing the N-Li bond, and the other The lithium atom forms a three-coordination mode with the oxygen atom in the three ligands; among them, the three ligands form positive monovalent ions with four lithium atoms, and the magnesium atom forms negative monovalent ions with three n-butyl groups.

[0020] The preparation method of the above-mentioned nitrogen-oxygen ion-containing lithium-magnesium bimetallic catalyst consists of the following steps:

[0021] 1) Preparation of N,N,O-tridentate amino alcohol ligand: under nitrogen protection, N,N-dimethylaniline (3.63g, 30mmol) and N,N,N',N'-tetramethyl Add ethylenediamine (...

Embodiment 2

[0026] Application of the nitrogen-oxygen-containing lithium-magnesium bimetallic catalyst in the reduction preparation of aldehyde compounds.

[0027] 1) The preparation of the nitrogen-oxygen ion-containing lithium-magnesium bimetallic catalyst is the same as in Example 1.

[0028] 2) Catalytic reduction of benzaldehyde to benzyl alcohol (MPV): under nitrogen protection at room temperature, benzaldehyde (4.0mmol) and isopropanol (4.8mmol) were added to nitrogen-containing oxygen-ion lithium-magnesium bimetallic catalyst (0.2 mmol), reflux and stir the reaction for 1 hour, then terminate the reaction with water, extract with ether, dry, and after rotary evaporation, separate with column chromatography (the mobile phase is a mixed solvent of n-hexane and ethyl acetate of 7:3), After concentration, it becomes benzyl alcohol. Yield 97%. 1 H NMR (300MHz, CDCl 3 ): δ (ppm) 3.62 (s, 1H, OH), 4.55 (s, 2H, CH2), 6.86-7.39 (m, 5H, C 6 h 5 ).

Embodiment 3

[0030] Application of the nitrogen-oxygen-containing lithium-magnesium bimetallic catalyst in the reduction preparation of ketone compounds.

[0031] 1) The preparation of the nitrogen-oxygen ion-containing lithium-magnesium bimetallic catalyst is the same as in Example 1.

[0032] 2) Catalyzing the reduction of acetophenone to 1-phenylethanol (MPV): under the protection of nitrogen at room temperature, add acetophenone (4.0 mmol) and isopropanol (4.8 mmol) to the nitrogen-containing oxygen ion lithium magnesium bismuth Metal (0.2mmol), after reflux and stirring for 1 hour, then stop the reaction with water, extract with ether, dry, and after rotary evaporation, separate by column chromatography (the mobile phase is a mixture of n-hexane and ethyl acetate at 7:3 solvent), which is 1-phenylethanol after concentration, and the yield is 94%. 1 H NMR (300MHz, CDCl 3 ): δ (ppm) 1.48 (d, 3H, CH3), 3.62 (s, 1H, OH), 4.65 (s, H, CH), 7.13-7.45 (m, 5H, C 6 h 5 ).

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Abstract

The invention relates to a nitrogen and oxygen ion containing lithium and magnesium bimetallic catalyst and a preparation method thereof and application thereof and belongs to the technical field of bimetallic catalysts. According to the nitrogen and oxygen ion containing lithium and magnesium bimetallic catalyst, technical problems, in an existing catalyst used in the MPV reaction, that the structure is complicated, the preparation is uneasy, the catalyst activity is not high enough, the usage is large and the reaction time is long are mainly solved. According to the technical scheme, the preparation method of the nitrogen and oxygen ion containing lithium and magnesium bimetallic catalyst comprises the following steps of 1) preparing a N, N, O-tridentate alkamine ligand: preparing the N,N, O-tridentate alkamine ligand according to the prior art; and 2) preparing the nitrogen and oxygen ion containing lithium and magnesium bimetallic catalyst: under the atmosphere of nitrogen, usingn-butyllithium to to remove hydrogen from the N, N, O-tridentate alkamine ligand in ethyl ether solution at 0 degree centigrade; after the solution recovers to the room temperature, stirring the solution for 1-2 hours; and then slowly dripping 0.5 equivalents of dibutyl magnesium into the solution at 0 degree centigrade; continuing to stir the solution for 4-6 hours; after the reaction is finished, filtering a reaction solution; concentrating a filter liquor in a vacuum state to separate out colorless and transparent crystals, wherein the colorless and transparent crystals are the nitrogen andoxygen ion containing lithium and magnesium bimetallic catalysts.

Description

technical field [0001] The invention relates to a nitrogen-oxygen ion-containing lithium-magnesium bimetallic catalyst and a preparation method and application thereof, belonging to the technical field of bimetallic catalysts. Background technique [0002] The Meerwein-Ponndorf-Verley (MPV) reaction is a reduction reaction for the preparation of primary and secondary alcohols with high selectivity and high efficiency. The catalysts commonly used in this reaction all have complex structures, are difficult to prepare, have insufficient catalyst activity, consume large amounts, and have long reaction times. Therefore, the development of new and efficient catalysts is still the focus of research on this reaction. The current literature reports are all alkoxides, oxides and their complexes centered on a single metal. Bimetallic compounds are considered to be potential high-efficiency catalysts because they contain two different metal centers and can show synergistic properties ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/22C07C209/00C07C211/65C07C29/14C07C33/20C07C29/143C07C33/22
CPCB01J31/2217B01J2231/643B01J2531/11C07C29/14C07C29/143C07C211/65C07C2601/14C07C33/20C07C33/22
Inventor 华宇鹏上官灵芝庞晶琳
Owner 鄂尔多斯应用技术学院
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