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Hypnone preparation method

A technology of acetophenone and ethylbenzene is applied in the application field of organic synthesis and achieves the effects of high yield, reduced environmental hazards and simple synthesis method

Inactive Publication Date: 2009-02-11
EAST CHINA NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] So far, there is no one-step synthesis of organically modified SBA15 as a carrier to load W 10 o 32 4- , to obtain a catalyst with a large specific surface area

Method used

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Embodiment 1: Catalyst SBA15-NH 3 -W 10 o 32 Synthesis of (II): After 2g P123 (Aldrich) is completely dissolved in 65ml of deionized water, add 10ml of concentrated hydrochloric acid (37.5%), stir and heat to 40°C in a water bath, then add 4.5ml of orthosilicate ethyl ester, After hydrolysis for 1 hour, 0.3 mL of APTES (Fluka) was added, stirred at 40°C for 20 hours, crystallized at 96°C for 24 hours, cooled, suction filtered, and dried. Weigh 1.5g of white solid and add it to 400ml of 95% ethanol (AR), reflux at 70°C for 24h, filter with suction, wash with ethanol and deionized water, dry, record as SBA15-NH 2 1 . Weigh 0.75g of SBA15-NH 2 1 Add to 10ml of CH 2 Cl 2 In, add 0.35g (2.3mmol) of CF 3 SO 3 After H(Alfa), stir for 8h, filter, and use 15ml of dichloromethane (CH 2 Cl 2 ), ethanol (ETOH), ether (ETOET) washing, vacuum drying at room temperature for 3h. Weigh 0.8g of (n-Bu 4 N) 4 W 10 o 32 Dissolve with 15ml of acetonitrile (CH 3 CN), after c...

Embodiment 2

[0022] Embodiment 2: 0.1g catalyst A, 13ml volume ratio is that acetonitrile and water of 3:0.5 are solvent, the ethylbenzene of 0.2ml (1.7mmol) joins in the quartz reactor of 50ml, feeds the O of 5mlmin-1 , stir Half an hour later, a 500W high-pressure mercury lamp (dominant wavelength: 365nm) was turned on for 6 hours of light, dried with anhydrous magnesium sulfate, centrifuged and sampled, and detected by GC.

Embodiment 3

[0023]Embodiment 3: 0.1g catalyst A, 13ml volume ratio is that the acetonitrile and water of 2:1 are solvent, the ethylbenzene of 0.2ml (1.7mmol) joins in the quartz reactor of 50ml, feeds the O of 5mlmin-1 , stir Half an hour later, a 500W high-pressure mercury lamp (dominant wavelength: 365nm) was turned on for 6 hours of light, extracted with ethyl acetate, centrifuged and sampled, and detected by GC.

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Abstract

The invention relates to a method of preparing acetophenone by ethylbenzene photocatalysis and oxidation, belonging to the technical field of organic synthesis application. The method is that under the condition of using acetonitrile and water with a certain volume ratio as solvent, photocatalysis and oxidation is carried out on ethylbenzene by the loaded W10O32<4-> catalyst to prepare acetophenone. The invention has the advantages that the method is simple, the synthesis time is short, the reaction is operated under normal temperature and pressure and is easy to be operated, the selectivity of product acetophenone is up to 98 percent, and the yield of acetophenone is high. No corrosive waste liquor appears during the reaction process, meanwhile, the catalyst activity and the performance for repeated use are improved, the use of organic solvent is reduced, and the harm to environment is reduced.

Description

technical field [0001] The invention relates to a method for preparing acetophenone by photocatalytic oxidation of ethylbenzene, more specifically, under the condition that acetonitrile and water in a certain volume ratio are used as solvents, using loaded W 10 o 32 4- A catalyst photocatalytically oxidizes ethylbenzene to prepare acetophenone, which belongs to the technical field of organic synthesis application. Background technique [0002] Acetophenone is an important organic synthesis intermediate, which is widely used in the manufacture of spices, drugs and other organic synthesis raw materials. It can also be used as a solvent for cellulose ethers, cellulose esters and resins, and for plasticizing plastics, etc. agent has broad application prospects. [0003] There are many traditional methods for synthesizing acetophenone, and the most commonly used method is generally the use of Friedel-Crafts homogeneous reaction, that is, the reaction of benzene with acetyl chl...

Claims

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Application Information

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IPC IPC(8): C07C49/78C07C45/36B01J29/00
Inventor 杨平倪伶俐吕媛种彦利
Owner EAST CHINA NORMAL UNIVERSITY