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A kind of magnetic pentacoordinate mononuclear cobalt complex and its synthesis method and application

A technology of cobalt complexes and synthesis methods, which is applied in the direction of organic compound/hydride/coordination complex catalysts, cobalt organic compounds, organic chemical methods, etc., and can solve the problems of insufficient catalyst activity, long reaction time, and difficulty in preparation, etc. , to achieve good industrial application prospects, short reaction time, and easy-to-obtain raw materials

Active Publication Date: 2022-04-22
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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  • A kind of magnetic pentacoordinate mononuclear cobalt complex and its synthesis method and application
  • A kind of magnetic pentacoordinate mononuclear cobalt complex and its synthesis method and application
  • A kind of magnetic pentacoordinate mononuclear cobalt complex and its synthesis method and application

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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, a synthesis method and an application thereof, belonging to the technical field of catalyst preparation. The purpose of the invention is to solve the technical problems of complex structure, difficult preparation, insufficient catalyst activity, large dosage and long reaction time of existing catalysts. The technical solution adopted in the present invention is that the synthesis steps are: under the protection of an inert gas, the ether solution of tetramethylethylenediamine is added to cyclohexanone after n-butyllithium lithiation, and after stirring for 1-2 hours Slowly add anhydrous cobalt chloride into the acetone bath, return to room temperature and stir for 2-4 hours. After the reaction is completed, the filtrate is concentrated in vacuo, and a purple transparent crystal is precipitated, which is a magnetic pentacoordinated mononuclear cobalt complex. The compound synthesized by the present invention is prepared by "one-pot method", the preparation process is simple, the raw materials are easy to obtain, and the reaction conditions are mild; as a catalyst, it has high selectivity to the MPV reaction of aldehydes and ketones, and can efficiently synthesize the corresponding of 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 Patents(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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