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3:1 type mg/li bimetallic catalyst and its preparation method and application

A technology for bimetallic catalysts and catalysis of aldehydes, applied in the direction of physical/chemical process catalysts, catalytic reactions, chemical instruments and methods, etc., can solve the problems of insufficient catalyst activity, complex catalyst structure, long reaction time, etc., and achieve catalytic reaction time The effect of short, high yield and simple preparation process

Inactive Publication Date: 2019-05-17
SHANXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

MPV reactions usually use metal compounds such as main group metals, transition metals, lanthanides and actinides as catalysts, mainly monometallic alkoxides, oxides and their complexes, etc., and the catalyst has a complex structure, is not easy to prepare, and has insufficient catalyst activity. High, large dosage, long reaction time, etc.

Method used

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  • 3:1 type mg/li bimetallic catalyst and its preparation method and application
  • 3:1 type mg/li bimetallic catalyst and its preparation method and application
  • 3:1 type mg/li bimetallic catalyst and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Example 1 Preparation of 3:1 type N, N, O-tridentate Mg / Li bimetallic catalyst

[0017] Slowly drop n-butyllithium (29.20 mL, 2.5 M, n-hexane solution) into the ether solution of TMEDA (11.02 g, 73 mmol) at 0°C, return to room temperature and react for 2 hours, then add cyclohexanone (7.54 mL, 73mmol) was dropped into the above-mentioned reaction solution to continue the reaction for 2 hours, then hydrolyzed under acidic conditions, and the aqueous phase obtained after liquid separation was neutralized to weak alkalinity with 5% aqueous sodium hydroxide solution, then extracted three times with anhydrous ether, organic The phase was dried with anhydrous magnesium sulfate and distilled under reduced pressure, and the colorless fraction at 78°C was collected to obtain the N,N,O-tridentate aminoalcohol ligand with a yield of 84%;

[0018] Under the protection of an inert gas, the N,N,O-tridentate aminoalcohol ligand (2.0mmol, 0.43g) was dissolved in 10mL of ether solvent, ...

Embodiment 2

[0021] (1) the preparation of catalyst is the same as embodiment 1

[0022] Catalytic reduction of benzaldehyde to benzyl alcohol (MPV): under nitrogen protection at room temperature, benzaldehyde (0.42g, 4.0mmol) and isopropanol (0.37mL, 4.8mmol) were added to a nitrogen-protected 3:1 type N,N, In the O-tridentate Mg / Li bimetallic catalyst (1.06g, 0.2mmol), after reflux stirring reaction for 1 hour, then terminate the reaction with water, extract with ether, dry, after rotary evaporation, separate with column chromatography (mobile phase 7:3 mixed solvent of n-hexane and ethyl acetate), benzyl alcohol after concentration. Yield 94%. 1 HNMR (300MHz, CDCl 3 ): δ(ppm)3.62(s,1H,OH),4.55(s,2H,CH 2 ),6.86-7.39(m,5H,C 6 h 5 ).

Embodiment 3

[0024] (1) the preparation of catalyst is the same as embodiment 1

[0025] (2) Catalytic reduction of acetophenone to 1-phenylethanol (MPV): under nitrogen protection at room temperature, acetophenone (0.48g, 4.0mmol) and isopropanol (0.37mL, 4.8mmol) were added to nitrogen-protected 3 : Type 1 N, N, O-tridentate Mg / Li bimetallic catalyst (1.06g, 0.2mmol), reflux and stir the reaction for 1 hour, then stop the reaction with water, extract with ether, dry, rotary evaporate, and use column Separation by chromatography (the mobile phase is a 7:3 mixed solvent of n-hexane and ethyl acetate), and concentrated to 1-phenylethanol with a yield of 91%. 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 provides a 3:1 type Mg / Li bimetallic catalyst, a preparation method therefor and an application of the 3:1 type Mg / Li bimetallic catalyst. The preparation method for the catalyst comprises the steps: (1) preparing an N,N,O-trident alkamine ligand; and (2) under the conditions of inert gas protection and ice water bath, dropwise adding a 1.5-times amount of n-butyl lithium into an ether solution of alkamine, dropwise adding a 0.5-time amount of dibutyl magnesium into the obtained reaction solution, then, dripping a 0.5-time amount of aqueous ether solution, carrying out filtrating after the reaction is completed, and carrying out vacuum concentration on the filtrate, so as to separate out colorless transparent crystals. The preparation method for the catalyst is simple and convenient and is low in condition requirements, non-transition metals, i.e. lithium and magnesium which are cheap and are low in toxicity are used as catalytic active metals, an Meerwein-Ponndorf-Verley (MPV) reaction for preparing corresponding first-level and second-level alcoholic compounds through reducing different types of aldehyde and ketone compounds has relatively high selectivity and catalytic activity, and the catalytic reaction is short in time and high in yield, so that the catalyst has a very good industrial application prospect.

Description

technical field [0001] The invention relates to a bimetallic catalyst, in particular to a 3:1 type N,N,O-tridentate Mg / Li bimetallic and its preparation method and application. Background technique [0002] The selective synthesis of primary and secondary alcohols is an important transformation process in fields such as organic synthesis, pharmaceutical and food flavor industries. The Meerwein-Ponndorf-Verley (MPV) reaction is considered to be one of the important reactions for the preparation of primary and secondary alcohols from aldehydes and ketones. It usually uses a system of hydrogen donors, strong bases and catalysts, and the most important part is high efficiency. catalyst. Therefore, the development of new and efficient catalytic reaction systems is still the focus of scientific research workers. MPV reactions usually use metal compounds such as main group metals, transition metals, lanthanides and actinides as catalysts, mainly monometallic alkoxides, oxides and...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/22C07F19/00C07C33/22C07C29/143
CPCB01J31/2213B01J31/2217B01J2231/643B01J2531/0205B01J2531/0241B01J2531/11B01J2531/22C07C29/143C07F3/003C07F3/02C07C33/22
Inventor 魏学红华宇鹏郭志强
Owner SHANXI UNIV
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