Method for synthesizing edible flavor lenthionine

Abstract

The invention relates to a method for synthesizing edible flavor lenthionine. The method comprises the following steps of: performing a thio-reaction between sodium tetrathiocarbonate and methylene diiodide in absolute ethyl alcohol, extracting by using carbon tetrachloride, drying and distilling to obtain the finished product. The lenthionine (also called as 1,2,3,4,5,6- pentathiacycloheptane) is widely applied to sauce products, meat products, convenience food and flavoring broth series; the fragrance is pure, real, strong and mellow; the lenthionine has full meat taste and good taste, can cover unpleasant smell and can resist high temperature; and the lenthionine is an ideal selection for canned mushrooms, mushroom sauces, convenience food and flavorings and has broad market prospects.

Description

technical field

[0001] The invention belongs to the field of fine chemical industry, and relates to a method for synthesizing edible spice shiitake essence, that is, 1,2,3,5,6-pentathiacycloheptane. Background technique

[0002] In today's society, people's choice of food is becoming 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 edible spices is increasing day by day. Shiitake mushroom is one of the internationally recognized health vegetables, which can improve human immune function. Lentinus edodes 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 have aroused great interest. However, the traditional method for synthesizing 1,2,3,5,6-pentat...

Examples

Embodiment 1

[0021] A kind of synthetic method of 1,2,3,5,6-pentathiocycloheptane, concrete operation steps are as follows:

[0022] Raw material ratio:

[0023] Sodium tetrathiocarbonate 186g

[0024] Diiodomethane 186g

[0025] Absolute ethanol 1400g

[0026] Carbon tetrachloride 900g

[0027] Anhydrous Calcium Chloride Appropriate amount

[0028] Steps:

[0029] (1) Thio: Add 186g sodium tetrathiocarbonate and 400g absolute ethanol in a three-necked reaction flask equipped with a stirrer, a constant pressure dropping funnel, and a thermometer until sodium tetrathiocarbonate is completely dissolved. In 2 hours, add the dehydrated ethanol solution of diiodomethane dropwise with a constant pressure dropping funnel (dissolve 186g of diiodomethane in 1000g of dehydrated ethanol in a beaker in advance), after dropping, keep stirring at a constant temperature of 25°C for 10 Hour;

[0030] (2) Extraction: the above-mentioned reaction solution is diluted with 2000g of water, then extracte...

Embodiment 2

[0033] A kind of synthetic method of 1,2,3,5,6-pentathiocycloheptane, concrete operation steps are as follows:

[0034] Raw material ratio:

[0035] Sodium tetrathiocarbonate 192g

[0036] Diiodomethane 190g

[0037] Absolute ethanol 1450g

[0038] Carbon tetrachloride 900g

[0039] Anhydrous Calcium Chloride Appropriate amount

[0040] Steps:

[0041] (1) Thio: Add 192g of sodium tetrathiocarbonate and 450g of absolute ethanol in a three-necked reaction flask equipped with a stirrer, a constant pressure dropping funnel, and a thermometer until sodium tetrathiocarbonate is completely dissolved. Add the dehydrated ethanol solution of diiodomethane dropwise with a constant pressure dropping funnel within 2 hours (dissolve 190g of diiodomethane in 1000g of dehydrated ethanol in a beaker in advance), and stir the reaction at a constant temperature of 25°C for 10 Hour;

[0042] (2) Extraction: the above-mentioned reaction solution is diluted with 2000g of water, then extract...

Embodiment 3

[0045] A method for synthesizing 1,2,3,5,6-pentathiocycloheptane, the specific operation steps are as follows.

[0046] Raw material ratio:

[0047] Sodium tetrathiocarbonate 198g

[0048] Diiodomethane 200g

[0049] Absolute ethanol 1600g

[0050] Carbon tetrachloride 900g

[0051] Anhydrous Calcium Chloride Appropriate amount

[0052] Steps:

[0053] (1) Thio: Add 198g sodium tetrathiocarbonate and 500g absolute ethanol in a three-necked reaction flask equipped with a stirrer, a constant pressure dropping funnel, and a thermometer until sodium tetrathiocarbonate is completely dissolved. Add the dehydrated ethanol solution of diiodomethane dropwise with a constant pressure dropping funnel within 2 hours (dissolve 200g of diiodomethane in 1100g of dehydrated ethanol in a beaker in advance), and stir the reaction at a constant temperature of 25°C for 10 Hour;

[0054] (2) Extraction: the above-mentioned reaction solution is diluted with 2000g of water, then extracted thr...

technical field

[0001] The invention belongs to the field of fine chemical industry, and relates to a method for synthesizing edible spice shiitake essence, that is, 1,2,3,5,6-pentathiacycloheptane. Background technique

[0002] In today's society, people's choice of food is becoming 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 edible spices is increasing day by day. Shiitake mushroom is one of the internationally recognized health vegetables, which can improve human immune function. Lentinus edodes 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 have aroused great interest. However, the traditional method for synthesizing 1,2,3,5,6-pentat...

Examples

Embodiment 1

[0021] A kind of synthetic method of 1,2,3,5,6-pentathiocycloheptane, concrete operation steps are as follows:

[0022] Raw material ratio:

[0023] Sodium tetrathiocarbonate 186g

[0024] Diiodomethane 186g

[0025] Absolute ethanol 1400g

[0026] Carbon tetrachloride 900g

[0027] Anhydrous Calcium Chloride Appropriate amount

[0028] Steps:

[0029] (1) Thio: Add 186g sodium tetrathiocarbonate and 400g absolute ethanol in a three-necked reaction flask equipped with a stirrer, a constant pressure dropping funnel, and a thermometer until sodium tetrathiocarbonate is completely dissolved. In 2 hours, add the dehydrated ethanol solution of diiodomethane dropwise with a constant pressure dropping funnel (dissolve 186g of diiodomethane in 1000g of dehydrated ethanol in a beaker in advance), after dropping, keep stirring at a constant temperature of 25°C for 10 Hour;

[0030] (2) Extraction: the above-mentioned reaction solution is diluted with 2000g of water, then extracte...

Embodiment 2

[0033] A kind of synthetic method of 1,2,3,5,6-pentathiocycloheptane, concrete operation steps are as follows:

[0034] Raw material ratio:

[0035] Sodium tetrathiocarbonate 192g

[0036] Diiodomethane 190g

[0037] Absolute ethanol 1450g

[0038] Carbon tetrachloride 900g

[0039] Anhydrous Calcium Chloride Appropriate amount

[0040] Steps:

[0041] (1) Thio: Add 192g of sodium tetrathiocarbonate and 450g of absolute ethanol in a three-necked reaction flask equipped with a stirrer, a constant pressure dropping funnel, and a thermometer until sodium tetrathiocarbonate is completely dissolved. Add the dehydrated ethanol solution of diiodomethane dropwise with a constant pressure dropping funnel within 2 hours (dissolve 190g of diiodomethane in 1000g of dehydrated ethanol in a beaker in advance), and stir the reaction at a constant temperature of 25°C for 10 Hour;

[0042] (2) Extraction: the above-mentioned reaction solution is diluted with 2000g of water, then extract...

Embodiment 3

[0045] A method for synthesizing 1,2,3,5,6-pentathiocycloheptane, the specific operation steps are as follows.

[0046] Raw material ratio:

[0047] Sodium tetrathiocarbonate 198g

[0048] Diiodomethane 200g

[0049] Absolute ethanol 1600g

[0050] Carbon tetrachloride 900g

[0051] Anhydrous Calcium Chloride Appropriate amount

[0052] Steps:

[0053] (1) Thio: Add 198g sodium tetrathiocarbonate and 500g absolute ethanol in a three-necked reaction flask equipped with a stirrer, a constant pressure dropping funnel, and a thermometer until sodium tetrathiocarbonate is completely dissolved. Add the dehydrated ethanol solution of diiodomethane dropwise with a constant pressure dropping funnel within 2 hours (dissolve 200g of diiodomethane in 1100g of dehydrated ethanol in a beaker in advance), and stir the reaction at a constant temperature of 25°C for 10 Hour;

[0054] (2) Extraction: the above-mentioned reaction solution is diluted with 2000g of water, then extracted thr...