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1,1,3,3-tetraalkylguanidine carbonyl cobalt metal organic ionic liquid and its preparation method and application

A technology of tetraalkylguanidine and ionic liquid, which is applied to 1,1,3,3-tetraalkylguanidine carbonyl cobalt metal organic ionic liquid and its preparation and application fields, so as to improve the utilization rate, reduce the production cost and the technological process. easy effect

Active Publication Date: 2018-12-28
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the easy decomposition of cobalt carbonyl itself leads to many difficulties in directly recovering and reusing cobalt carbonyl in the form of cobalt carbonyl after the reaction. Therefore, recycling and reusing cobalt carbonyl catalysts has always been the focus and difficulty of many researchers.

Method used

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  • 1,1,3,3-tetraalkylguanidine carbonyl cobalt metal organic ionic liquid and its preparation method and application
  • 1,1,3,3-tetraalkylguanidine carbonyl cobalt metal organic ionic liquid and its preparation method and application
  • 1,1,3,3-tetraalkylguanidine carbonyl cobalt metal organic ionic liquid and its preparation method and application

Examples

Experimental program
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Effect test

Embodiment 1

[0044] Preparation of 1,1,-Dimethyl-3,3-diethylguanidinecarbonyl cobalt metal organic ionic liquid (catalyst a)

[0045] Under N2 protection, KOH (6 mmol) and Co 2 (CO) 8 (1 mmol), then added 6 mL of THF treated with anhydrous and anaerobic treatment, and stirred thoroughly for 2 h. After the reaction was completed, the supernatant was transferred to another Schlenk reaction tube, and then 3 mmol of 1 was added to the Schlenk reaction tube. ,1,-Dimethyl-3,3-diethylguanidine hydrochloride was fully stirred and reacted for 5h. After the reaction was completed, the THF solvent was vacuumed off, and then 6mL of anhydrous and anaerobic treated CH 2 Cl 2 Solution, dissolve and filter to remove precipitate, vacuum remove CH 2 Cl 2 Solvent to obtain the corresponding 1,1,-dimethyl-3,3-diethylguanidine cobalt carbonyl metal organic ionic liquid catalyst a.

[0046] Replace the raw material 1,1,3,3-tetraalkylguanidine hydrochloride with 1,1,-dimethyl-3,3-di-n-butylguanidine di-n-bu...

Embodiment 2

[0049] In an autoclave with a volume of 50 mL, add 3 mL of absolute ethanol, 5 mmol of propylene oxide (Propylene oxide), 2 mol% of 1,1,3,3-tetraalkylguanidine carbonyl cobalt metal organic Ionic Liquid Catalysts a. Seal the reactor, replace the reactor with carbon monoxide 3 times, and seal the reactor. In the Schlenk vacuum line, the reaction system was replaced three times with carbon monoxide gas at room temperature, the pressure of CO gas was filled at 7.0 MPa, and the temperature was slowly raised to 60 by the temperature controller. o C, reacted for 24 hours, cooled to room temperature, unloaded, the liquid obtained by the reaction was carried out qualitative analysis with Agilent 6890 / 5973 gas chromatography spectrometer, and Agilent 7890 gas chromatography was used for quantitative analysis, the conversion rate of propylene oxide was 77%, 3- Ethyl hydroxybutyrate selectivity 90%.

Embodiment 3

[0051] In an autoclave with a volume of 50 mL, add 3 mL of absolute ethanol, 5 mmol of propylene oxide, and 2 mol% of 1,1,3,3-tetraalkylguanidine carbonyl cobalt metal organic ionic liquid catalyst b. Seal the reactor, replace the reactor with carbon monoxide 3 times, and seal the reactor. In the Schlenk vacuum line, the reaction system was replaced three times with carbon monoxide gas at room temperature, the pressure of CO gas was filled at 7.0 MPa, and the temperature was slowly raised to 60 by the temperature controller. o C, reacted for 24 hours, cooled to room temperature, unloaded the kettle, carried out qualitative analysis with Agilent 6890 / 5973 GC-MS, and quantitative analysis with Agilent 7890 gas chromatography, the conversion rate of propylene oxide was 50%, and the 3-hydroxyl Ethyl butyrate selectivity 91%.

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Abstract

The invention discloses a 1,1,3,3-tetra alkyl guanidine carbonyl cobalt metal organic ion liquid. A structure formula of the ion liquid is shown in the description. The invention also discloses a preparation method of the ion liquid and application of the ion liquid in synthesizing of 3-hydroxy carboxylate by epoxy compound hydroesterification. The 1,1,3,3-tetra alkyl guanidine carbonyl cobalt metal organic ion liquid has the advantages that guanidine cation has the double functions of stabilizing tetra carbonyl cobalt cation and using as a Lewis acid to activate epoxy compound primer; compared with the traditional Co2(CO)8 / azacycle catalytic system, the use of a nitrogen-containing organic matter is avoided; the ion liquid can be recycled and repeatedly used, the use rate of carbonyl cobalt is improved, and the production cost is reduced; the stability of the 1,1,3,3-tetra alkyl guanidine carbonyl cobalt metal organic ion liquid is high, the ion liquid can be repeatedly applied to catalysis of epoxy compound hydroesterification for multiple times, the catalytic reaction effect is good, and the separation and recycling are convenient.

Description

technical field [0001] The invention relates to a 1,1,3,3-tetraalkylguanidine carbonyl cobalt metal organic ionic liquid, a preparation method thereof and an application in synthesizing 3-hydroxy carboxylate by hydroesterification of epoxy compounds. Background technique [0002] 3-Hydroxycarboxylates are a class of stable and important bifunctional platform compounds, which can be further converted into important organic intermediates and polyester raw materials such as diketones and 1,3-diols, and then widely used in organic fine chemistry Drugs, medicinal chemistry, agricultural chemistry and other fields. Traditional synthetic methods mainly include the Reformatsky reaction of aldehydes or ketones with α-halogenated esters, the reduction reaction of β-ketoesters catalyzed by chemical or biological methods, and the esterification reaction of 3-hydroxycarboxylic acids and esters. Expensive, harsh reaction conditions, low product yield, many side reactions, difficult produ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C277/08C07C279/04C07D295/215B01J31/20C07C67/37C07C69/675C07C69/732C07C69/734C07C69/736
CPCB01J31/0279B01J31/0282B01J31/20B01J2531/845C07C67/37C07C277/08C07C279/04C07D295/215C07C69/675C07C69/732C07C69/734C07C69/736
Inventor 刘建华张伟夏春谷童进
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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