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Method for preparing raspberry ketone in acidic ionic liquid

A technology for acidic ionic liquid and raspberry ketone, which is applied in the field of preparing raspberry ketone in acidic ionic liquid and preparing raspberry ketone, can solve the problems of toxic and harmful catalysts, non-recyclable use, use of volatile organic solvents, industrial three wastes, and the like, To achieve the effect of simple reaction process and easy operation

Active Publication Date: 2012-07-18
HIGH & NEW TECH RES CENT OF HENAN ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a new green method for preparing raspberry ketone in order to solve the problems in the prior art that the catalysts are poisonous and harmful and cannot be recycled, use volatile organic solvents and produce a large amount of industrial waste.

Method used

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  • Method for preparing raspberry ketone in acidic ionic liquid

Examples

Experimental program
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Effect test

Embodiment 1

[0017] Put 0.6 mole of phenol, 0.8 mole of butenone and 0.2 mole of [NMPH]H into the reaction vessel 2 PO 4 Acidic ionic liquid, stirred and reacted at 30°C for 12 hours. Heating to 90°C, adding 2 moles of water. The product raspberry ketone was obtained by filtration and separation, and the yield of the reaction was 32%; the unreacted raw materials and isolated liquid could be used for the next experiment after dehydration.

Embodiment 2

[0019] Put 0.6 mole of phenol, 0.5 mole of butenone and 0.2 mole of [NMPH]HSO into the reaction vessel 4 Acidic ionic liquid, stirred and reacted at 40°C for 12 hours. Heating to 90°C, adding 2 moles of water. The product raspberry ketone was obtained by filtration and separation, and the reaction yield was 40%. The unreacted raw materials and ionic liquid could be used in the next experiment after dehydration.

Embodiment 3

[0021] 0.4 mole of phenol, 0.5 mole of butenone and 0.2 mole of [NMPH]PTSA acidic ionic liquid were put into the reaction vessel, and stirred and reacted at 15° C. for 24 hours. Heated to 90°C and added 1 mole of water. The product raspberry ketone was obtained by filtration and separation, and the reaction yield was 34%; the unreacted raw materials and ionic liquid could be used for the next experiment after dehydration.

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Abstract

The invention discloses a method for preparing raspberry ketone in acidic ionic liquid and belongs to the field of organic chemical synthesis. The raspberry ketone is synthesized by performing a selective addition reaction on phenol and butanone which serve as initial raw materials and the acidic ionic liquid, which is high in thermal stability and difficult to volatilize, can be recycled and serves as a catalyst and a reaction solvent. According to the method, any organic solvent which is easy to volatilize and an additionally added catalyst are not used, the reaction condition is mild, and the post treatment is simple and convenient, so the method is a green and environment-friendly new method for synthesizing the raspberry ketone. The problems that the catalyst is toxic and harmful and cannot be recycled, a volatile organic solvent is used, and a large number of industrial three wastes are produced in the prior art are solved.

Description

technical field [0001] The invention relates to a method for preparing raspberry ketone, in particular to a method for preparing raspberry ketone in an acidic ionic liquid, and belongs to the field of organic chemical synthesis. Background technique [0002] Raspberry ketone (p-hydroxybutyrophenone), also known as rubus ketone, is a spice with elegant fruity aroma widely used at home and abroad. It can be used as a food additive in beverages, candies, biscuits, and snacks; it can also be used as a Modifier, used in jasmine, tuberose and other fragrances or cosmetics. [0003] There are two traditional methods for synthesizing raspberry ketone. The first method uses p-hydroxybenzaldehyde and acetone as raw materials, undergoes condensation reaction and hydrogenation reduction reaction to obtain raspberry ketone (CN1097729). The reaction conditions of this method are relatively harsh, and strong bases and expensive transition metals are required as catalysts. The catalysts ar...

Claims

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Application Information

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IPC IPC(8): C07C49/245C07C45/69
CPCY02P20/54
Inventor 郭辉张国宝庄玉伟王颖曹健郭晓战
Owner HIGH & NEW TECH RES CENT OF HENAN ACAD OF SCI
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