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A method for preparing aldehydes or ketones by air oxidation of alcohols with alumina as a co-catalyst

A co-catalyst, alumina technology, applied in physical/chemical process catalysts, carbon-based compound preparation, chemical instruments and methods, etc., can solve the problems of unsafe, high pressure, inconvenient use, etc., and achieve easy control of operation and conversion. The effect of high rate and mild reaction conditions

Inactive Publication Date: 2016-08-17
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, as can be seen from the examples given in the above-mentioned patent applications, the TEMPO / bromine (or active bromine) / NaNO used 2 The characteristics and effects of the oxidation system that catalyzes molecular oxygen: the use of sodium nitrite, halogen bromine or active bromine is inconvenient and unsafe, the pressure used is relatively high, and organic solvents are used

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] In a 100mL single-necked bottle, put magneton, 3mmol benzyl alcohol, 3mol% TEMPO, 2mol% copper bromide and 0.8g neutral alumina into the single-necked bottle together, and seal the bottle mouth with plastic wrap (preservative film left with holes). Start the powerful magnetic stirrer at the bottom of the one-necked bottle for stirring, and start timing. After the reaction was finished, the organic matter was extracted with ethyl acetate, the organic phase was washed with water and brine respectively, and then dried with anhydrous magnesium sulfate, and then the organic phase was analyzed by GC (the conversion rate of benzyl alcohol was 100%, and the selectivity of benzaldehyde was 100%. %), and finally, the product was washed through a 300-400 mesh silica gel column, and the yield of benzaldehyde was 92%.

Embodiment 2

[0026] In a 100 mL polytetrafluoroethylene stainless steel autoclave, put magnets, 3mmol benzyl alcohol, 3mol% TEMPO, 2mol% copper bromide and 0.8g neutral alumina into the autoclave together, and feed oxygen to 0.2MPa, then seal it. Start the strong magnetic stirrer at the outer bottom of the kettle to stir, adopt the external oil bath heating method, control the heating rate and reaction temperature by the temperature measurement controller, and start timing when the set temperature is 80°C; during the reaction process, if the pressure drops , that is, oxygen supplementation. After the reaction was finished, the organic matter was extracted with ethyl acetate, the organic phase was washed with water and brine respectively, and then dried with anhydrous magnesium sulfate, and then the organic phase was analyzed by GC (the conversion rate of benzyl alcohol was 100%, and the selectivity of benzaldehyde was 100%. %), and finally, the product was washed through a 300-400 mesh si...

Embodiment 3

[0028] The method of operation is the same as in Example 2, except that the neutral aluminum oxide is changed to the aluminum oxide that has been oxidized once, and reused for the second time. The conversion rate of benzyl alcohol is 100%, and the selectivity of benzaldehyde is 100%. Yield 88%.

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PUM

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Abstract

A catalytic system using alumina as a cocatalyst, a new method for efficient and highly selective air oxidation of alcohols to aldehydes or ketones, in the absence of solvents, nitrogen-containing ligands, and alkalis, according to the substrate 3 mmol benzyl alcohol 2~3 mol% of 2,2,6,6-tetramethylpiperidine nitroxide as the main catalyst, 1~2 mol% of copper salt, 0.8~1 g of alumina, oxygen or air pressure 0.1~0.5 MPa, the reaction temperature is 20~80°C, the reaction time is 1~24 hours, the conversion rate of benzyl alcohol is 100%, the selectivity of product benzaldehyde is 100%, and the yield is 92%. The invention is a simple catalytic system with high activity, low price, simple and easy operation, mild catalytic reaction conditions, easy separation and reuse of alumina, no pollution, and easy industrial production. good way.

Description

technical field [0001] The present invention relates to a kind of Al 2 o 3 , TEMPO and CuBr 2 The invention is a new catalytic system, a method for preparing aldehydes and ketones by catalytic air oxidation of alcohols with high efficiency and high selectivity, and specifically relates to a method for efficiently and selectively oxidizing alcohols into aldehydes or ketones by using air or oxygen as an oxidant. Background technique [0002] The selective oxidation of alcohols to carbonyl compounds is one of the important functional group conversion reactions in organic synthesis, and this type of reaction occupies a very important position in the field of basic research and fine organic synthesis. The oxidation of alcohols to the corresponding carbonyl compounds exceeds one million tons every year in the world, and the selective oxidation of alcohols has become a permanent topic in the field of chemical research. Most of the oxidation uses inorganic oxidants such as: chrom...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C45/38C07C47/54C07C47/232C07C47/277C07C47/24B01J31/30B01J31/28
CPCY02P20/582
Inventor 王秋芬郑庚修赵晶晶杨倩姜守相许燕战付旭
Owner UNIV OF JINAN