Method for preparing edible essence 8-mercaptomenthone from pulegone and sodium sulfide

A technology of mercaptohormone and menthone, applied in the field of food 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

[0008] The technical problem mainly solved by the present invention is to provide a kind of 8-mercaptomaleic acid with low production cost, fully utilized reaction raw materials, high product purity, and suitable for industrial production Synthetic method of ketone to overcome low yield and pollution and poisoning problems of hydrogen sulfide method

Method used

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  • Method for preparing edible essence 8-mercaptomenthone from pulegone and sodium sulfide
  • Method for preparing edible essence 8-mercaptomenthone from pulegone and sodium sulfide
  • Method for preparing edible essence 8-mercaptomenthone from pulegone and sodium sulfide

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Add 300 grams of menthone, 250 grams of sodium sulfide and 1000 grams of water into the reactor, stir and mix evenly, heat to 60° C. to 70° C., and react for 15 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 280 g of crude 8-mercaptomaleone.

[0024] Add 280 grams of 8-mercaptomaleone crude product in 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 dry the filtered solid to constant weight to obtain the final product 8 -170 grams of mercaptomaleone, the yield is 46%, which is better than the bibliographical reports of the existing normal pressure reaction.

[0025] The NMR parameters of the prepared 8-mercaptomaleone are:

[0026] 1 H-NMR(300MHz,DMSO)δ:...

Embodiment 2

[0029] Add 300 grams of menthone, 280 grams of sodium sulfide and 1000 grams of methanol into the reactor, stir and mix evenly, heat to 60°C~70°C, add 5g of zinc chloride (Friedel-Crafts catalyst), and react under constant stirring 15 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.

[0030] Add 320 grams of 8-mercaptomaleone crude product in the reaction vessel, then add 400 grams of ethanol to reflux for 4 hours, then cool the solution to room temperature, separate out the solid, then filter, and dry the filtered solid to constant weight to obtain the final product 8 -240 grams of mercaptomaleone, the yield is 65%.

Embodiment 3

[0032] Add 300 grams of menthone, 320 grams of sodium sulfide and 1200 grams of ethanol into the reactor, stir and mix evenly, heat to 60° C. to 70° C., and react for 15 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 290 g of crude 8-mercaptomaleone.

[0033] Add 290 grams of 8-mercaptomaleone crude product in 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 dry the filtered solid to constant weight to obtain the final product 8 - 200 grams of mercaptomaleone, the yield is 54%.

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Abstract

The invention relates to a method for preparing edible essence 8-mercaptomenthone from pulegone and sodium sulfide. The method utilizes sodium sulfide, potassium sulfide or ammonium sulfide as a raw material. Compared with the prior art, the method does not use toxic gas H2S, is free of multiple complicated processes, has high operation safety and is environmentally friendly. The method has a high 8-mercaptomenthone yield, simple processes and mild reaction conditions, is suitable for industrial production and solves the problems of a low yield of the prior art.

Description

technical field [0001] The invention relates to a method for preparing food flavor 8-mercaptomaleone by using menthone and sodium sulfide, and 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 synthet...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C323/22C07C319/04
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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