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Method for synthesizing lactone compound by catalytic oxidation of cyclone

A catalytic oxidation and oxidation technology, applied in chemical instruments and methods, chemical/physical processes, physical/chemical process catalysts, etc., can solve the problems of small reaction TON, low catalytic efficiency, and low repeatability, and achieve low cost, Effect of high catalytic activity and simplified homogeneous process

Inactive Publication Date: 2008-04-16
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this catalyst system has not been used in the research of other lactones, and the reproducibility is not high. Although the conversion rate and selectivity of the oxidation reaction of cyclohexanone BV can reach 100%, the reaction TON is small and the catalytic efficiency is low.
In addition, due to the lack of relevant research, the author has not tried the influence of other metal oxides on the reaction, especially the influence of the catalyst's basic strength on the catalytic activity has not been reported so far.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Embodiment 1: the preparation of metal oxide MgO: with 0.056mol Mg (NO 3 ) 2 ·6H 2 O dissolved in 10 mL H 2 O, stirred at 10°C to obtain a clear solution, and added dropwise a volume fraction of 2.5% NH 3 ·H 2 O adjusts pH=8. Stirring was continued for 1 h, the resulting white suspension was crystallized at room temperature for 6 h, and suction filtered. The obtained product was washed successively with distilled water and ethanol, dried, and calcined at 400° C. for 2 h in an air atmosphere to obtain the catalyst. The reaction conditions adopted for the synthesis of lactones are: 0.0029mol cyclohexanone, 2.4mL molar ratio of 1:0.5 benzonitrile and 1,4-dioxane mixed solution, 0.9mL of 10%H 2 o 2 , control the bath temperature to 313K, and react for 2 hours. Record it as 1#. After the reaction is completed, the analysis results are shown in Table 1.

Embodiment 2

[0017] Embodiment 2: composite metal oxide MgO / SnO 2 (9:1) preparation: 0.056 mol Mg(NO 3 ) 2 ·6H 2 O and 0.018mol SnCl 4 .5H 2 O dissolved in 20 mL H 2 O, stirred at 20°C to obtain a clear solution, and added dropwise a volume fraction of 2.5% NH 3 ·H 2 O adjusts pH=10. Stirring was continued for 3 h, the resulting white suspension was crystallized at room temperature for 9 h, and suction filtered. The obtained product was washed successively with distilled water and ethanol, dried, and calcined at 500° C. for 4 hours in an air atmosphere to obtain the catalyst. The reaction conditions adopted are: 0.0029mol cyclohexanone, 2.4mL molar ratio is 1: 1.0 mixed solution of benzonitrile and 1,4-dioxane, 1.2mL of 20%H 2 o 2 , control the bath temperature to 323 K, and react for 4 hours. Record it as 2#. After the reaction is completed, the analysis results are shown in Table 1.

Embodiment 3

[0018] Embodiment 3: composite metal oxide MgO / SnO 2 (8:2) preparation: 0.056mol Mg(NO 3 ) 2 ·6H 2 O and 0.021mol SnCl 4 .5H 2 O dissolved in 30 mL H 2 O, stirred at 30°C to obtain a clear solution, and added dropwise a volume fraction of 2.5% NH 3 ·H 2 O adjusts pH=10. Stirring was continued for 5 h, the resulting white suspension was crystallized at room temperature for 10 h, and suction filtered. The obtained product was washed successively with distilled water and ethanol, dried, and calcined at 600° C. for 6 hours in an air atmosphere to obtain the catalyst. The reaction conditions adopted are: 0.0029mol cyclohexanone, 2.4mL molar ratio is 1: 1.5 mixed solution of benzonitrile and 1,4-dioxane, 1.8mL of 30%H 2 o 2 , control the bath temperature to 333 K, and react for 6 hours. Write it down as 3#. After the reaction is completed, the analysis results are shown in Table 1.

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PUM

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Abstract

The present invention belongs to chemistry technology field, in particular to a method to synthesize lactone compound with cyclone oxide which is an environmental friendly catalyst. The present invention adopts a composite metal oxide MgO / SnO2compound as the catalyst, adopts hydrogen peroxide as the oxidant, and Benzonitrile together with 1,4-bensodioxanes as the solvents, then the cyclone oxide is catalyzed to synthesize the lactone compound in a specific reaction temperature. The present invention uses ketone adamantine, cyclohexanone, and cyclopentanone available in the market, and the yield can be as high as 90 percent in the mild condition. Meanwhile, because of the hydrogen peroxide adopted ad the oxidant, the oxidation methods in prior art is avoided such as peracid, all of which cause environmental problem, and the aim of environmental friendly catalyzing / conversion is accomplished. The present invention is low in price, but has suitability for industrialized production of lactone compound.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to an environmentally friendly method for synthesizing lactone compounds by catalytically oxidizing cyclic ketones with aqueous hydrogen peroxide solution. Background technique [0002] The Baeyer-Villiger (BV) oxidation reaction is an important class of reactions that oxidize cyclic ketones or chain ketones into lactones or esters. In view of the fact that this reaction can control the stereostructure of the product, the conversion of functional groups and ring formation in organic synthesis Expansion matters. The oxidant used in the traditional BV oxidation reaction is generally a peroxyacid (such as trifluoroperoxyacetic acid, peroxybenzoic acid, m-chloroperoxybenzoic acid, etc.). The oxidants used are all chemical oxidants. These oxidants have some general disadvantages, such as serious environmental pollution, large acid pollution, large amount of three w...

Claims

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Application Information

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IPC IPC(8): C07D315/00C07D309/30C07D493/08B01J23/14B01J23/02
Inventor 戴维林李静霞范康年
Owner FUDAN UNIV
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