Magnetic pentacoordinate mononuclear cobalt complex, and synthesis method and application thereof

A technology of cobalt complexes and synthesis methods, applied in organic compound/hydride/coordination complex catalysts, cobalt organic compounds, organic chemical methods, etc., can solve the problems of insufficient catalyst activity, long reaction time, complex structure, etc. , to achieve the effect of good industrial application prospect, short reaction time and simple preparation process

Active Publication Date: 2020-03-24
鄂尔多斯应用技术学院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to solve the technical problems of existing catalysts such as complex structure, difficult preparation, insufficient catalyst activity, large dosage and long reaction time, and provide a magnetic pentacoordinated mononuclear cobalt complex and its synthesis method and application

Method used

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  • Magnetic pentacoordinate mononuclear cobalt complex, and synthesis method and application thereof
  • Magnetic pentacoordinate mononuclear cobalt complex, and synthesis method and application thereof
  • Magnetic pentacoordinate mononuclear cobalt complex, and synthesis method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] A kind of magnetic pentacoordinate mononuclear cobalt complex in the present embodiment, the structural formula of this complex is:

[0019]

[0020] In the formula: the cobalt atom forms a five-coordinate structure with two oxygen atoms, two nitrogen atoms and chlorine atoms in the ligand, and forms two five-membered rings sharing the N-Co bond, and the cobalt atom and the two ligands are respectively Oxygen atoms form a dimer molecular structure with Co-O coordination bonds.

[0021] The synthesis method of the above-mentioned magnetic pentacoordinated mononuclear cobalt complex is as follows: under the protection of an inert gas, slowly drop n-butyllithium (29.20mL, 2.5M, n-hexane solution) into tetramethyl Ethylenediamine (TMEDA) (11.02g, 73mmol) was reacted in ether solution for 2 hours, then cyclohexanone (7.54mL, 73mmol) was dripped into the above reaction solution to continue the reaction for 2 hours, and anhydrous Cobalt chloride (9.41g, 73mmol) was returne...

Embodiment 2

[0024] The structural formula of the complex in this example is the same as that in Example 1.

[0025] The synthesis steps are as follows: under the protection of inert gas, slowly drop n-butyllithium (29.20mL, 2.5M, n-hexane solution) into the ether solution of tetramethylethylenediamine (TMEDA) (70mmol) at 0°C to react After 2 hours, cyclohexanone (70mmol) was dripped into the above-mentioned reaction solution to continue the reaction for 2 hours, anhydrous cobalt chloride (70mmol) was slowly added under an acetone bath, and room temperature was restored to stir for 4 hours. After the reaction was completed, the filtrate was concentrated in vacuo. Purple transparent crystals were precipitated, namely the pentacoordinate mononuclear cobalt catalyst, with a yield of 73% and a melting point of 142-145°C.

Embodiment 3

[0027] The structural formula of the complex in this example is the same as that in Example 1.

[0028] The synthesis steps are as follows: under the protection of inert gas, slowly drop n-butyllithium (29.20mL, 2.5M, n-hexane solution) into the ether solution of tetramethylethylenediamine (TMEDA) (75mmol) at 0°C to react After 2 hours, cyclohexanone (75mmol) was dripped into the above-mentioned reaction solution to continue the reaction for 2 hours, anhydrous cobalt chloride (75mmol) was slowly added under an acetone bath, and room temperature was restored to stir for 4 hours. After the reaction was completed, the filtrate was concentrated in vacuo. Purple transparent crystals were precipitated, namely the pentacoordinate mononuclear cobalt catalyst, with a yield of 73% and a melting point of 142-145°C.

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Abstract

The invention relates to a magnetic pentacoordinate mononuclear cobalt complex, and a synthesis method and application thereof, belonging to the technical field of catalyst preparation. The inventionaims to solve the technical problems of complex structure, difficulty in preparation, low activity, large consumption and long reaction time of conventional catalysts. According to a technical schemein the invention, the method comprises the following synthesis steps of: under the protection of inert gas, subjecting an ether solution of tetramethylethylenediamine to lithiation by n-butyllithium and then to addition with cyclohexanone, slowly adding anhydrous cobalt chloride an acetone bath after a stirring reaction for 1-2 hours, performing stirring at room temperature for 2-4 hours, subjecting a filtrate to vacuum concentration after the reaction is completed, and allowing purple transparent crystals to be precipitated so as to obtain the magnetic pentacoordinate mononuclear cobalt complex. The synthesized complex is prepared by adopting a one-pot method; preparation process is simple; raw materials are easy to obtain; the reaction conditions are mild; and the complex used as a catalyst has high selectivity for MPV reactions of aldehyde and ketone compounds, and can be used for efficiently synthesizing corresponding alcohol compounds.

Description

technical field [0001] The invention relates to a magnetic pentacoordinate mononuclear cobalt complex, a synthesis method and an application thereof, belonging to the technical field of catalyst preparation. 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. This reaction usually uses metal compounds such as main group metals, transition metals, lanthanides and actinides as catalysts , mainly metal alkoxides, oxides and their complexes, etc., and the catalyst has a complex structure, is not easy to prepare, the catalyst activity is not high enough, the dosage is large, and the reaction time is long. Therefore, it is necessary to develop a new and e...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F15/06B01J31/22C07C29/143C07C33/22
CPCC07F15/065C07C29/143B01J31/2217C07B2200/13B01J2231/643B01J2531/845C07C33/22
Inventor 华宇鹏庞晶琳康敏燕高艳鹏
Owner 鄂尔多斯应用技术学院
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