Preparation method of edible essence 8-mercaptomenthone

A kind of sulfhydryl horse, synthesis method technology, applied in the field of edible flavor preparation

Inactive Publication Date: 2014-10-22
南京誉佳医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The technical problem mainly solved by the present invention is to provide a kind of production cost is low, and reaction raw material utilizes fully, and product purity is high, and is suitable for industrialized production 8-mercaptomaleone Synthetic method to overcome the low yield and pollution and poisoning problems of hydrogen sulfide method

Method used

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  • Preparation method of edible essence 8-mercaptomenthone
  • Preparation method of edible essence 8-mercaptomenthone
  • Preparation method of edible essence 8-mercaptomenthone

Examples

Experimental program
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Effect test

Embodiment 1

[0021] Add 300 grams of menthol, 250 grams of sodium polysulfide and 1000 grams of water into the reactor, stir and mix evenly, heat to 80°C to 90°C, and react for 12 hours under constant stirring. Then the above reaction mixture was diluted with water, acidified to neutral with hydrochloric acid, cooled to room temperature, filtered, and the filter cake was washed with warm water at a temperature of 35° C. to 40° C. to obtain 310 g of crude 8-mercaptomaleone.

[0022] Add 310 grams of crude 8-mercaptomaleone into the reaction vessel, then add 400 grams of ethanol to reflux for 4 hours, then cool the solution to room temperature, precipitate a solid, then filter, and vacuum-dry the filtered solid to constant weight to obtain the final product 195 grams of 8-mercaptomaleone, the yield is 52.4%, which is better than the bibliographical reports of the existing normal pressure reaction.

[0023] The NMR parameters of the prepared 8-mercaptomaleone are:

[0024] 1 H-NMR(300MHz,DM...

Embodiment 2

[0027] Add 300 grams of menthol, 330 grams of sodium polysulfide and 1000 grams of methanol into the reactor, stir and mix evenly, heat to 80°C to 90°C, and react for 12 hours under constant stirring. Then the above reaction mixture was diluted with water, acidified to neutral with hydrochloric acid, cooled to room temperature, filtered, and the filter cake was washed with warm water at a temperature of 35° C. to 40° C. to obtain 305 g of crude 8-mercaptomaleone.

[0028] Add 305 grams of crude 8-mercaptomaleone into the reaction vessel, then add 400 grams of ethanol to reflux for 4 hours, then cool the solution to room temperature, precipitate a solid, then filter, and vacuum-dry the filtered solid to constant weight to obtain the final product 210 grams of 8-mercaptomaleone, the yield is 56.5%.

Embodiment 3

[0030] Add 300 grams of menthone, 400 grams of sodium polysulfide and 1200 grams of ethanol to the reactor, stir and mix evenly, heat to 80 ° C ~ 90 ° C, add 5 g of zinc chloride (Friedel-Crafts catalyst), under constant stirring React for 12 hours. Then the above reaction mixture was diluted with water, acidified to neutral with hydrochloric acid, cooled to room temperature, filtered, and the filter cake was washed with warm water at a temperature of 35° C. to 40° C. to obtain 320 g of crude 8-mercaptomaleone.

[0031] Add 320 grams of crude 8-mercaptomaleone into the reaction vessel, then add 400 grams of ethanol to reflux for 4 hours, then cool the solution to room temperature, precipitate a solid, then filter, and vacuum-dry the filtered solid to constant weight to obtain the final product 220 grams of 8-mercaptomaleone, the yield is 59%.

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Abstract

The invention discloses a preparation method of edible essence 8-mercaptomenthone. The preparation method utilizes polysulfides and pulegone as raw materials. Compared with the prior art, the preparation method is free of toxic H2S use and multiple complicated processes and has high operation safety and environmental friendliness. The preparation method has a high 8-mercaptomenthone yield, simple processes and mild reaction conditions and is suitable for industrial production.

Description

technical field [0001] The invention relates to a method for preparing food flavor 8-mercaptomaleone by using menthone, which belongs to the technical field of food flavor preparation. Background technique [0002] Essence, as a special high-concentration additive that can affect the taste and flavor of food, has been widely used in various fields of food production. It can make up for the fragrance defects of food itself, endow some foods with vivid original taste, enhance the fragrance of food, and cover up the flavor of food. These advantages of essence make it increasingly become the focus of people's research. With the development of modern analysis technology and the continuous improvement of analysis methods, more and more structures of aroma substances have been identified, especially after the discovery of small but indispensable ingredients such as sulfur compounds, synthetic essences The aroma is closer to the natural flavor, so that the synthetic flavor industr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C323/22C07C319/06
Inventor 梁承远宋慧慧江桂林陈雪峰
Owner 南京誉佳医药科技有限公司
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