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Synthetic method of edible spice 1,2,3,5,6-pentathiocycloheptane

A technology of pentathiocycloheptane and edible spices, applied in the direction of organic chemistry, which can solve the problems of harsh reaction conditions, many operation steps, and long reaction time, and achieve the effect of good taste, simple process operation, and pure aroma

Inactive Publication Date: 2011-11-30
TIANJIN CHEM REAGENT RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional method for synthesizing 1,2,3,5,6-pentathiacycloheptane has harsh reaction conditions, the low temperature reaches -78°C, many operating steps, multiple extractions and separations are required, and the reaction time is long and the yield is low. Low

Method used

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  • Synthetic method of edible spice 1,2,3,5,6-pentathiocycloheptane

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Experimental program
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Effect test

Embodiment 1

[0020] A kind of synthetic method of flavoring 1,2,3,5,6-pentathiacycloheptane, concrete operation steps are as follows:

[0021] Raw material ratio:

[0022]

[0023] Steps:

[0024] (1) Thio: Add 188g of sodium tetrathiocarbonate and 400ml of absolute ethanol into a three-necked reaction flask equipped with a stirrer, a constant pressure dropping funnel, and a thermometer until the sodium tetrathiocarbonate is completely dissolved. Add the absolute ethanol solution of diiodomethane dropwise with a constant pressure dropping funnel within 2 hours, and then stir and react at a constant temperature of 25°C for 10 hours after dropping;

[0025] The treatment method of diiodomethane before use is: dissolve 188g of diiodomethane in 1000ml of absolute ethanol in a beaker;

[0026] (2) Extraction: Dilute the above reaction solution with 2000ml of water, then extract three times with cyclohexane, separate the water layer and combine the extract, add an appropriate amount of anh...

Embodiment 2

[0029] A kind of synthetic method of flavoring 1,2,3,5,6-pentathiacycloheptane, concrete operation steps are as follows:

[0030] Raw material ratio:

[0031]

[0032] Steps:

[0033] (1) Thio: Add 190g of sodium tetrathiocarbonate and 450ml of absolute ethanol into a three-necked reaction flask equipped with a stirrer, a constant pressure dropping funnel, and a thermometer until the sodium tetrathiocarbonate is completely dissolved. In 2 hours, add the dehydrated ethanol solution of diiodomethane dropwise with a constant pressure dropping funnel (dissolve 196g of diiodomethane in 1100ml of dehydrated ethanol in a beaker in advance), and stir the reaction at a constant temperature of 25°C for 10 Hour.

[0034] (2) Extraction: Dilute the above reaction solution with 2000ml of water, then extract three times with cyclohexane, separate the water layer and combine the extracts, add an appropriate amount of anhydrous calcium chloride to dry.

[0035] (3) Distillation: filter...

Embodiment 3

[0037] A kind of synthetic method of flavoring 1,2,3,5,6-pentathiacycloheptane, concrete operation steps are as follows:

[0038] Raw material ratio:

[0039]

[0040] Steps:

[0041] (1) Thio: Add 195g of sodium tetrathiocarbonate and 500ml of absolute ethanol into a three-necked reaction flask equipped with a stirrer, a constant pressure dropping funnel, and a thermometer until the sodium tetrathiocarbonate is completely dissolved. Add the dehydrated ethanol solution of diiodomethane dropwise with a constant pressure dropping funnel within 2 hours (dissolve 198g of diiodomethane in 1100ml dehydrated ethanol in a beaker in advance), and keep stirring at a constant temperature of 25°C for 10 Hour.

[0042] (2) Extraction: Dilute the above reaction solution with 2000ml of water, then extract three times with cyclohexane, separate the water layer and combine the extracts, add an appropriate amount of anhydrous calcium chloride to dry.

[0043] (3) Distillation: filter the...

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Abstract

The present invention relates to a kind of synthetic method of food spice 1,2,3,5,6-pentathiocycloheptane, the steps are as follows: firstly thiating: in a three-necked reaction flask equipped with a stirrer, a constant pressure dropping funnel, and a thermometer Add sodium tetrathiocarbonate and absolute ethanol to the mixture and stir until sodium tetrathiocarbonate is completely dissolved. Add the absolute ethanol solution of diiodomethane dropwise with a constant pressure dropping funnel within 2 hours at 25°C. Stir and react at a constant temperature of 25°C for 10 hours; second extraction: dilute the above reaction solution with water, then extract three times with cyclohexane, separate the water layer and combine the extracts, add anhydrous calcium chloride for drying; finally obtain the finished product by distillation. The invention provides an edible spice 1,2,3,5,6-pentathiacycloheptane with strong characteristic fragrance, good antibacterial activity and biological activity. The process is simple and the yield is high, and it can be safely used as a spice in It is a new type of mushroom flavor during frying, frying, cooking, frying and other cooking processes.

Description

technical field [0001] The invention belongs to the field of fine chemicals, in particular to a method for synthesizing 1,2,3,5,6-pentathiacycloheptane, an edible spice. technical background [0002] In today's society, people's choice of food is more and more colorful. In addition to caring about their nutritional value, they also pay great attention to their color, aroma and taste. Therefore, the demand for food spices is increasing day by day. [0003] Shiitake mushroom is one of the internationally recognized health vegetables, which can improve human immune function. 1,2,3,5,6-Pentathiocycloheptane is the main aroma component of Lentinus edodes. It is the first organic compound containing multiple sulfur atoms obtained from nature. It has a strong characteristic aroma and good antibacterial activity and biological activity. . [0004] At present, the preparation method of existing 1,2,3,5,6-pentathiocycloheptane is as follows: prepare sodium tetrathiocarbonate (yield ...

Claims

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Application Information

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IPC IPC(8): C07D341/00
Inventor 赵德章张序红
Owner TIANJIN CHEM REAGENT RES INST
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