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Preparation method for acetophenone

A technology of acetophenone and methyl styrene, which is applied in the preparation of organic compounds, chemical instruments and methods, and carbon-based compounds. It can solve the problems of low catalyst reuse rate and high catalyst preparation cost, and achieve short synthesis time , high selectivity and yield, simple method

Inactive Publication Date: 2009-08-05
EAST CHINA NORMAL UNIV
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  • Abstract
  • Description
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AI Technical Summary

Problems solved by technology

The cost of catalyst preparation required for this type of photochemical reaction is high and the catalyst reuse rate is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Add 0.2ml of α-methylstyrene and 20ml of acetonitrile into the photoreactor device, stir, pass condensed water, the flow rate of oxygen is 2ml / min, turn on the 125w medium pressure mercury lamp, the reaction time is 0.5 hours, add toluene as internal Standard, as GC analysis, the productive rate of acetophenone is 2.79%, selectivity is 79.68%.

Embodiment 2

[0017] Add 1.5ml of α-methylstyrene and 40ml of acetonitrile into the photoreactor device, stir, pass condensed water, the flow rate of oxygen is 8ml / min, turn on the 125w medium pressure mercury lamp, the reaction time is 2 hours, and the added toluene makes The internal standard was analyzed by GC, and the yield of acetophenone was 6.44%, and the selectivity was 67.89%.

Embodiment 3

[0019] Add 1.5ml of α-methylstyrene and 40ml of acetonitrile into the photoreactor device, stir, pass condensed water, the flow rate of oxygen is 8ml / min, turn on the 125w medium pressure mercury lamp, the reaction time is 3 hours, and the added toluene makes The internal standard was analyzed by GC, and the yield of acetophenone was 41.63%, and the selectivity was 74.49%.

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Abstract

The invention relates to a preparation method of hypnone, in particular to a method for preparing hypnone by direct photooxidation under the condition with Alpha-vinyltoluene and without catalyst. The invention belongs to the technical field of organic synthesis application. The Alpha-vinyltoluene and acetonitrile with the volume ratio of 1: (0.4 to 100) are put into a light reactor and stirred. The hypnone is prepared after putting through condensed water into a reactor casing and adjusting the flow rate, maintaining reaction temperature to be room temperature, inletting oxygen into the reactor with the flow rate of 2 to 15ml / min, lighting a 125w medium pressure mercury lamp and reacting for 0.5 to 20 hour(s). The method can be used for synthesizing hypnone directly at room temperature without catalysts so as to reduce synthesis cost; furthermore, the method has the advantages of less toxicity and being environment protective.

Description

technical field [0001] The invention relates to a method for preparing acetophenone, in particular to a method for preparing acetophenone by direct photooxidation of α-methylstyrene under the condition of no catalyst, and belongs to the technical field of organic synthesis application. Background technique [0002] Acetophenone is a commonly used organic product. As an important intermediate, it can be used to make toilet soap and cigarettes. It can also be used as a solvent for cellulose ethers, cellulose esters and resins, and a plasticizer for plastics. It has a wide range of applications. application prospects. [0003] There are many traditional methods for the synthesis of acetophenone. Mainly use benzene as raw material, utilize Friedel-Crafts homogeneous reaction, such as: benzene and acetic anhydride synthesize acetophenone under the catalysis of anhydrous aluminum trichloride, or use benzene, acetic anhydride and ethyl acetate as raw materials, in the absence of ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C45/36C07C49/78
Inventor 单永奎薛燕董健媛孔爱国杨帆
Owner EAST CHINA NORMAL UNIV
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