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Method for microwave synthesis of alpha-hydroxyacetophenone series compounds

A technology for hydroxyacetophenone and microwave synthesis, which is applied to the preparation of carbon-based compounds, organic compounds, chemical instruments and methods, etc., can solve problems that have not been reported, shorten the reaction time, increase the reaction yield, and accelerate The effect of the reaction

Inactive Publication Date: 2009-11-18
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, the microwave synthesis method of phthalocyanine of the invention patent of National Tsinghua University (ZL patent No. 01129641.0), Li Yanlun et al. reported the synthesis of 5-benzylidene pseudohydantoin under microwave radiation (published in "Organic Chemistry" 2009 No. 3 issue), Guo Huanfang et al. reported microwave-promoted synthesis of oxartemisinin and its derivatives (published in "Chemistry Bulletin" 2009 No. 1), all of which are examples of microwave radiation applied to organic synthesis, but the use of microwaves to synthesize α- The method of hydroxyacetophenone series compounds has not been reported in China

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0007] Embodiment 1: microwave synthesis α-hydroxyacetophenone

[0008] Weigh 2.5mmol α-bromoacetophenone, add 50mL of deionized water into a microwave reactor with a pressure gauge, put the reactor into a microwave reactor, adjust the power of the microwave to maintain the pressure of the reaction system At 0.30MPa, microwave radiation for 40min, and then the reaction product was extracted twice with 50mL ethyl acetate, the organic layer was dried and concentrated, then subjected to gas chromatography analysis, and the content of the product α-hydroxyacetophenone was measured to be 89.8%.

Embodiment 2

[0009] Embodiment 2: microwave synthesis α-hydroxy p-methoxyacetophenone

[0010] Weigh 1.5mmol α-bromo-p-methoxyacetophenone, add 40mL of deionized water into a microwave reactor with a pressure gauge, put the reactor into a microwave reactor, and adjust the power of the microwave so that The pressure of the reaction system was maintained at 0.32MPa, microwave radiation was applied for 25min, and then the reaction product was extracted twice with 50mL ethyl acetate. The content is 96.2%.

Embodiment 3

[0011] Embodiment 3: microwave synthesis α-hydroxy m-chloroacetophenone

[0012] Weigh 3.0mmol α-bromo-m-chloroacetophenone, add 50mL of deionized water into a microwave reactor with a pressure gauge, put the reactor into a microwave reactor, adjust the power of the microwave, and make the reaction system The pressure was maintained at 0.30MPa, and microwave radiation was applied for 25min, then the reaction product was extracted twice with 50mL ethyl acetate, the organic layer was dried and concentrated, and then analyzed by gas chromatography, the content of the product α-hydroxy m-chloroacetophenone was measured to be 95.1 %.

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Abstract

The invention relates to a method for microwave synthesis of alpha-hydroxyacetophenone series compounds, which belongs to the technical field of organic synthesis. The method is a novel method and comprises the following steps: using alpha-bromoacetophenone series compounds and water as raw materials and placing the raw materials into a microwave reaction kettle, wherein the water also serves as a reaction medium; and under microwave radiation, synthesizing the alpha-hydroxyacetophenone series compounds through one step. The synthesis method is simple and quick, has high conversion rate, needs no organic media and catalysts, has no waste disposal and is environment-friendly. The method can greatly shorten the reaction time for synthesizing the alpha-hydroxyacetophenone series compounds and reduce the generation of byproducts, and is a high-efficiency and energy-saving environment-friendly synthesis method.

Description

technical field [0001] The invention discloses a method for synthesizing α-hydroxyacetophenone series compounds by microwave, belonging to the technical field of organic synthesis. Specifically, the α-bromoacetophenone series compounds and water are used as the reaction raw materials, and the water is used as the reaction medium at the same time. In the microwave reaction device, the α-hydroxyacetophenone series compounds are synthesized in one step after microwave radiation and a certain reaction pressure is maintained. Methods. Background technique [0002] α-Hydroxyacetophenone series compounds are important organic synthesis intermediates and flavor raw materials. The conventional chemical synthesis method is to react α-bromoacetophenone or its derivatives with anhydrous sodium acetate to generate α-acetoxyacetophenone or its derivatives, and then hydrolyze to obtain α-hydroxyacetophenone or its derivatives. However, this kind of reaction process is cumbersome and time...

Claims

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Application Information

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IPC IPC(8): C07B41/02C07C49/82C07C49/84C07C45/64C07C205/45C07C201/12B01J19/12
Inventor 刘湘袁为国陈海波潘争光
Owner JIANGNAN UNIV
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