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Raspberry ketone synthesis method

A raspberry ketone and synthetic method technology, applied in the direction of chemical instruments and methods, carbon-based compound preparation, organic compound preparation, etc., can solve the problems of large environmental pressure, serious environmental pollution, hidden dangers of product safety, etc., to reduce pollution , high reaction yield, simple post-treatment effect

Inactive Publication Date: 2014-04-16
ANHUI FENGLE PERFUME
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Both of the methods described in these two patents use petrochemical raw materials as the initial raw materials, which poses great hidden dangers in product safety and limits the scope of application
[0006] (2) After synthesizing anisyl acetone with natural raw material anisaldehyde, a large amount of Lewis acid is used to demethylate the synthesis route. The process yield is low, the three wastes are large, and the environmental pollution is serious
The methods described in these two patents will generate a large amount of acid wastewater, and HBr is highly corrosive to equipment and pollutes seriously, causing greater environmental pressure

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] This embodiment relates to a kind of synthetic method of raspberry ketone

[0025] Add 1 mol of anisyl acetone, 6 mol of potassium hydroxide and 10 mol of N,N-dimethylacetamide into a 2L four-necked round bottom flask, heat and stir until dissolved, then slowly add 2 mol of thioglycolic acid dropwise into the mixture, Stir the reaction well, transfer the mixture to a 2L autoclave, replace the air in the autoclave with nitrogen, control the pressure to 0.1MPa, and the temperature to 130°C, react for 24h, stop the reaction and cool to room temperature. After adding dilute acid to neutralize the system, add toluene to extract the oil-water mixture, wash the oil phase with water and dry it with anhydrous magnesium sulfate. The solvent toluene was distilled off under normal pressure, and then distilled under reduced pressure to collect the crude product. After the crude product was distilled and recrystallized with ethyl acetate, the product had a purity of 98.7% and a yiel...

Embodiment 2

[0028] This embodiment relates to a kind of synthetic method of raspberry ketone

[0029] Add 1 mol of anisyl acetone, 12 mol of potassium hydroxide and 22 mol of N,N-dimethylacetamide into a 2L four-neck round bottom flask, heat and stir until dissolved, then slowly add 10 mol of thioglycolic acid dropwise to the mixture, fully Stir the reaction, transfer the mixture to a 2L autoclave, replace the air in the autoclave with nitrogen, control the pressure to 2.0MPa, and the temperature to 170°C, react for 150h, stop the reaction and cool to room temperature. After adding dilute acid to neutralize the system, add toluene to extract the oil-water mixture, wash the oil phase with water and dry it with anhydrous magnesium sulfate. The solvent toluene was distilled off under normal pressure, and then distilled under reduced pressure to collect the crude product. After the crude product was distilled and recrystallized with ethyl acetate, the product had a purity of 98.0% and a yiel...

Embodiment 3

[0032] This embodiment relates to a kind of synthetic method of raspberry ketone

[0033] Add 1 mol of anisyl acetone, 7 mol of potassium hydroxide and 12 mol of N,N-dimethylacetamide into a 2L four-neck round bottom flask, heat and stir until dissolved, then slowly add 6.5 mol of thioglycolic acid dropwise into the mixture, After all the solids were dissolved, the mixture was transferred to a 2L autoclave, the air in the autoclave was replaced with nitrogen, the pressure was controlled at 0.15MPa, the temperature was 170°C, and the reaction was carried out for 77h, then the reaction was stopped and cooled to room temperature. After adding dilute acid to neutralize the system, add toluene to extract the oil-water mixture, wash the oil phase with water and dry it with anhydrous magnesium sulfate. The solvent toluene was distilled off under normal pressure, and then distilled under reduced pressure to collect the crude product. After the crude product was distilled and recrysta...

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PUM

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Abstract

The invention discloses a raspberry ketone synthesis method, which comprises the following steps: anisylacetone, potassa, N,N-dimethylacetamide are added into a dry four-mouth bottle equipped with a thermometer, a dropping hopper and a condenser tube, heated, dissolved and slowly dropwise added with a demethylation reagent under the agitation condition, and the solid are completely dissolved; a liquid mixture is transferred to an autoclave and is pressurized to react under the protection of inert gas; the liquid mixture subjected to the reaction is neutralized to be neutral, an oil phase is extracted, and crude raspberry ketone is prepared after decompression distillation; the crude raspberry ketone is dissolved with a dissolvent and then crystallized so as to obtain the pure raspberry ketone. According to the invention, the yield is 85.2 percent and the product purity is 98.5 percent; on the basis of keeping the high reaction yield, the raw material cost is effectively lowered, besides, a large amount of acid waste water are not generated, as a result, the pollutions to the environment isare reduced, and the large-scale industrial production and application of the raspberry ketone are facilitated.

Description

technical field [0001] The present invention mainly relates to a kind of synthetic method, relate in particular to a kind of synthetic method of raspberry ketone. Background technique [0002] Raspberry ketone is a kind of spice with elegant and fruity aroma. It is mainly used as a fixative and modifier, and has a good weight loss effect. In addition, it is also an insect attractant in agriculture. [0003] The synthetic method of raspberry ketone has following two kinds at present: [0004] (1) There are a variety of process routes for the synthesis of raspberry ketone from petrochemical raw materials. This process has abundant sources of raw materials, low price, few synthesis steps and high yield, but it usually cannot be used for the deployment of natural food flavors. [0005] For example, in patent CN93120105, a method for synthesizing raspberry ketone using p-hydroxybenzaldehyde as a raw material is disclosed, and in patent WO2009118755A2, a synthesis route using p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/245C07C45/64
CPCC07C45/64C07C49/245
Inventor 夏晋金劲松赵彬张勤朱俊峰张文张翼轸
Owner ANHUI FENGLE PERFUME
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