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Diosmin production method based on dimethylsulfoxide system

A technology of dimethyl sulfoxide and production methods, which is applied in the direction of chemical instruments and methods, sugar derivatives, sugar derivatives, etc., can solve problems such as large environmental pollution, and achieve short production cycle, low production cost, and reduced investment scale Effect

Inactive Publication Date: 2017-07-21
CHENGDU BETTER PHARMA TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is that the traditional diosmin production method causes great environmental pollution, and the purpose is to provide a diosmin production method based on a dimethyl sulfoxide system to solve the problem of large environmental pollution caused by the traditional diosmin production method

Method used

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] The diosmin production method based on the dimethyl sulfoxide system of the present invention comprises the following steps:

[0027] S1: Dissolve hesperidin and potassium iodide in dimethyl sulfoxide and put them into the first container, the ratio of the amount of potassium iodide to hesperidin is: 0.05-0.1:1.0, the hesperidin And the mass ratio with dimethyl sulfoxide is: 1.0-2.0:1.0;

[0028] S2: Add dimethyl sulfoxide and concentrated sulfuric acid into the second container, the mass ratio of dimethyl sulfoxide to hesperidin is 0.5:1.0, and the ratio of concentrated sulfuric acid to hesperidin is 0.1:1.0;

[0029] S3: The solution in the first container in step S1 and the solution in the second container in step S2 are fed and mixed into the reactor according to the volume ratio of the feed ratio of 2:1 to react, and the reaction temperature is 90-98 ° C, Cool down and collect the reaction solution after the reaction is complete;

[0030] S4: Transfer the reacti...

Embodiment 2

[0034] Based on Example 1, the mass ratio of potassium iodide to hesperidin in step S1 is 0.05:1.0, and the mass ratio of hesperidin to dimethyl sulfoxide is 1.0:1.0. Specifically include the following production steps:

[0035] (1) 12.5kg hesperidin and 0.17kg potassium iodide are dissolved in 12.5kg dimethyl sulfoxide and loaded into the A pump of the microreactor; (2) 6.25kg dimethyl sulfoxide is added to the B pump of the microreactor Sulfoxide and 0.2kg concentrated sulfuric acid; (3) Heat the reaction channel temperature of the microreactor to 90-98°C; (4) Adjust the feed ratio (volume: V / V) of the A pump and the B pump to 2:1 At the same time, the A pump and the B pump are turned on to mix and react, and the reaction residence time is controlled to be 6-10 seconds, and the temperature at the end of the reaction channel is controlled to 0-10°C to collect the reaction solution; In the reaction kettle, stir and control the temperature at 0-10°C, dropwise add methanol to p...

Embodiment 3

[0037] Based on Example 1, the mass ratio of potassium iodide to hesperidin in step S1 is 0.1:1.0, and the mass ratio of hesperidin to dimethyl sulfoxide is 2.0:1.0. The specific steps are as follows: (1) 12.5kg hesperidin and 0.34kg potassium iodide are dissolved with 6.25kg dimethyl sulfoxide and then loaded into the A pump of the microreactor; (2) 6.25 kg is added to the B pump of the microreactor. kg dimethyl sulfoxide and 0.2kg concentrated sulfuric acid; (3) heating the reaction channel temperature of the microreactor to 90-98°C; (4) adjusting the feed ratio (volume: V / V) of the A pump and the B pump 1 / 1, simultaneously turn on the A pump and the B pump to mix and react, and control the reaction residence time to be 6-10 seconds, and control the temperature at the end of the reaction channel to collect the reaction liquid at 0-10°C; Transfer the reaction solution to a reaction kettle, control the temperature at 0-10°C under stirring, add dropwise methanol to precipitate ...

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Abstract

The invention discloses a diosmin production method based on a dimethylsulfoxide system. The diosmin production method comprises the following steps that hesperidin and potassium iodide are dissolved with dimethyl sulfoxide and then are charged into a first container; the dimethyl sulfoxide and concentrated sulfuric acid are added into a second container; the solution inside the first container and the solution inside the second container are added into a reactor and are mixed for reaction, and the reaction solution is cooled and collected after reaction is completed; the collected reaction solution is transferred to a reaction kettle to obtain a wet diosmin product; the wet diosmin product is subjected to air blowing and drying at the temperature of 80 DEG C for 12 hours to obtain diosmin. A new diosmin production process is developed by combining the microreactor and a new dehydrogenation system (potassium iodide / sulfuric acid / dimethyl sulfoxide), the safety is good, the environment is not polluted, and the produced diosmin is high in purity and high in yield.

Description

technical field [0001] The invention relates to a method for producing diosmin, in particular to a method for producing diosmin based on a dimethyl sulfoxide system. Background technique [0002] Diosmin, also known as diosmin, molecular formula C28H32O15, CAS: 520-27-4. It is used to treat acute and chronic hemorrhoid attacks, and it can also be used for chronic venous insufficiency, such as varicose veins, edema of lower extremities, chronic ulcers of lower extremities, etc. The content of diosmin in plants is relatively small, so it is difficult to meet the huge demand of the market. Therefore, the production of diosmin is mainly obtained through synthetic methods. The content of hesperidin in Citrus aurantium is very large, depending on the place of origin and harvest season, the content of hesperidin is between 15-40%, and the structure of hesperidin and diomin is very similar, and diomin can pass through orange Dehydrogenation reaction of dermoside to obtain: [00...

Claims

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Application Information

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IPC IPC(8): C07H17/07C07H1/00
CPCC07H1/00C07H17/07
Inventor 黄清东杜琳张翔向世明杜伟
Owner CHENGDU BETTER PHARMA TECH CO LTD
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