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Microwave radiation ketone-nitrile condensation method adopting amine acetate catalysis

A technology of microwave radiation and ammonium acetate, applied in chemical instruments and methods, preparation of carboxylic acid nitrile, preparation of organic compounds, etc., can solve the problems of slow reaction and low yield, and achieve short reaction time, high efficiency and no solvent pollution effect

Inactive Publication Date: 2006-03-29
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The invention provides a method for ketone-nitrile condensation using microwave radiation catalyzed by ammonium acetate to overcome the shortcomings of low yield and slow reaction in the prior art

Method used

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  • Microwave radiation ketone-nitrile condensation method adopting amine acetate catalysis
  • Microwave radiation ketone-nitrile condensation method adopting amine acetate catalysis
  • Microwave radiation ketone-nitrile condensation method adopting amine acetate catalysis

Examples

Experimental program
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Effect test

Embodiment 1

[0013] This embodiment takes the condensation of benzophenone and malononitrile as an example.

[0014] Put 100 mg of benzophenone, equimolar amounts of malononitrile, and equimolar amounts of ammonium acetate into open dry glass test tubes to mix the reaction mixture thoroughly. Microwave for 3 minutes. After the reaction was completed, the reaction mixture was cooled. The cooled reaction mixture was fully dissolved in dichloromethane, and the ammonium acetate was removed using a suction filter funnel, and the dichloromethane suction filtrate was retained; the filtered ammonium acetate was washed twice with dichloromethane to fully collect the product. The above two dichloromethane solutions were combined, transferred to a round bottom flask, and the dichloromethane was removed by a rotary evaporator to obtain a crude product.

[0015] Finally, the obtained crude product was further separated and purified by silica gel column chromatography to obtain a ketone-nitrile conden...

Embodiment 2

[0017] This embodiment takes the condensation of fluorenone and malononitrile as an example.

[0018] Put 100 mg of fluorenone, equimolar amounts of malononitrile, and equimolar amounts of ammonium acetate into open dry glass test tubes to mix the reaction mixture thoroughly. Then, put the test tubes into a microwave oven and use a 300-watt microwave Radiation for 2 minutes. After the reaction was completed, the reaction mixture was cooled. Fully dissolve the cooled reaction mixture in dichloromethane, remove ammonium acetate using a suction filter funnel, retain the dichloromethane suction filtrate; and rinse the filtered ammonium acetate twice with dichloromethane. The above two dichloromethane solutions were combined. Transfer to a round bottom flask and remove the dichloromethane with a rotary evaporator to give the crude product.

[0019] Finally, the obtained crude product was recrystallized with ethanol, and the calculated yield of the ketone-nitrile condensation pro...

Embodiment 3

[0021] This embodiment This embodiment takes the condensation of acetophenone and malononitrile as an example.

[0022] Put 100 mg of acetophenone, equimolar amounts of malononitrile, and equimolar amounts of ammonium acetate into open dry glass test tubes to mix the reaction mixture thoroughly. Microwave irradiation for 1.5 minutes. After the reaction was completed, the reaction mixture was cooled. Fully dissolve the cooled reaction mixture in dichloromethane, remove ammonium acetate using a suction filter funnel, retain the dichloromethane suction filtrate; and rinse the filtered ammonium acetate twice with dichloromethane. The above two dichloromethane solutions were combined, transferred to a round bottom flask, and the dichloromethane was removed by a rotary evaporator to obtain a crude product.

[0023] Finally, the obtained crude product was further separated by silica gel column chromatography, and the calculated yield of the ketone-nitrile condensation product was 4...

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Abstract

The invention discloses a microwave radiation ketone-nitrile condensation method adopting amine acetate catalysis which comprises, charging malonic nitrile, fragrant ketone and acetic amine as catalyst by chemical measuring ration of the reaction, reacting 1-4 mins under the condition of 300-450W microwave radiation, the fragrant ketone includes any one of acetophenone, dibenzene ketone or fluorine ketone.

Description

Technical field: [0001] The invention belongs to the technical field of preparation methods of organic chemical ketone-nitrile condensates, in particular to a microwave radiation ketone-nitrile condensation method catalyzed by ammonium acetate. Background technique: [0002] The Knoevenagel condensation reaction of aromatic ketones and malononitrile is widely used in the production of various organic intermediates such as dyes and pharmaceuticals. According to "Organic Name Reaction (Volume Two)" (Chemical Industry Press, 1984, page 22 to page 28), traditional synthetic methods need to use a large amount of organic solvents and a long reaction time, and ketones occur The Knefnagel reaction is much more difficult than aldehydes, and the yields are very low. The use of solvents causes air pollution and increases the risk of fire. The equipment and motors used need to be explosion-proof, thus increasing the cost of equipment investment; the reaction time is too long, which wil...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C253/30C07C255/01
Inventor 程博
Owner UNIV OF SCI & TECH OF CHINA
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