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Method for synthesizing tetralone by liquid-phase catalytic oxidation of tetralin

A technology of tetralone and liquid phase catalysis, which is applied in the direction of chemical instruments and methods, oxidation preparation of carbonyl compounds, molecular sieve catalysts, etc., to achieve the effect of easy recovery, low equipment requirements and high conversion rate

Inactive Publication Date: 2009-01-07
YUNNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, no one has used mesoporous materials to catalyze the oxidation of tetralone to synthesize tetralone

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Sequentially weigh 1g of tetralin, 20mg of Co / MSiO 2 / MTiO 2Add the catalyst and 5ml of acetic acid into a 50ml three-necked flask, heat to 40°C, stir and slowly add 2ml of 30% H 2 o 2 , After 4 hours of reaction, stop the reaction, filter and separate. The sample was analyzed by gas spectrometer, the conversion rate of tetralone was 28.9%, the selectivity of tetralone was 62.3%, the selectivity of tetralone was 7.6%, and some phenols and acetic acid were esterified reaction, and a small amount of other by-products. Co / MSiO 2 / MTiO 2 Co-doped MSiO 2 / MTiO 2 .

Embodiment 2

[0030] Sequentially weigh 1g of tetralin and 120mg of Co / MSiO 2 / MTiO 2 Add the catalyst and 50ml of acetic acid into a 100ml three-necked flask, heat to 110°C, stir and slowly add 8ml of 30% H 2 o 2 , After 12 hours of reaction, stop the reaction, filter and separate. The sample was analyzed by gas spectrometer, the conversion rate of tetralone was 86.2%, the selectivity of tetralone was 68.6%, the selectivity of tetralone was 9.2%, and some phenols and acetic acid were esterified reaction, and a small amount of other by-products. Co / MSiO 2 / MTiO 2 Co-doped MSiO 2 / MTiO 2 .

Embodiment 3

[0032] Sequentially weigh 1g of tetralin and 100mg of Co / MSiO 2 / MTiO 2 Add the catalyst and 30ml of acetic acid into a 100ml three-necked flask, heat to 110°C, stir and slowly add 5ml of H 2 o 2 , After 8 hours of reaction, stop the reaction, filter and separate. The sample was analyzed by gas spectrometer, the conversion rate of tetralone was 92.3%, the selectivity of tetralone was 76.0%, the selectivity of tetralone was 3.5%, and some phenols and acetic acid were esterified reaction, and a small amount of other by-products. Co / MSiO 2 / MTiO 2 Co-doped MSiO 2 / MTiO 2 .

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PUM

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Abstract

The invention relates to a method for catalytically oxidizing tetrahydronaphthalene to tetralone in liquid phase. The invention relates to the synthesis method of ketone compounds, particularly the synthesis method of tetralone. The invention aims to develop a method for catalytically oxidizing tetrahydronaphthalene to tetralone in liquid phase at high conversion rate and high selectivity. The method selects a mesoporous material as a heterogeneous catalyst to catalytically oxidize tetrahydronaphthalene to tetralone under the condition of low temperature and liquid phase. The test result shows that the conversion rate of tetrahydronaphthalene is 97.6%, and the selectivity of tetralone is 75.5%.

Description

Technical field [0001] The present invention relates to the synthetic method of ketone compound, especially the synthetic method of tetralone. Background technique [0002] α-tetralone is an important biologically active organic intermediate, mainly used in insecticide carbaryl, antidepressant sertraline, anti-inflammatory, anti-rheumatic, anti-diabetic, anti- The synthesis of high blood pressure and other drugs is widely used in many fields such as pesticides, medicines, and adjuvants. Its traditional synthetic method is to take benzene and gamma-butyrolactone as raw materials under the action of acidic catalyst (such as aluminum trichloride) generation Friedel-Crafts acylation reaction synthesis [Chem.PhamBull., 1989; 37 (9): 2334- 2337; J.Am.Chem.Soc, 1952; 74:4721]; or use benzene and succinic anhydride as raw materials through acylation, reduction, cyclization and other multi-step synthesis [Liu University, Wang He, Journal of Ningxia University (Nature Science Editio...

Claims

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Application Information

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IPC IPC(8): C07C49/447C07C45/27B01J29/04B01J23/70B01J23/32B01J23/22
Inventor 王家强马永平翟中标
Owner YUNNAN UNIV
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