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A kind of preparation method of diosmin

A technology of diosmin and preparation steps, which is applied to the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve the problems of difficult recovery of iodine, increase of production costs, and health hazards of operators, and reduce high temperature The effect of impurity content, recovery rate improvement and purity improvement

Active Publication Date: 2019-04-30
NANJING CHIA TAI TIANQING PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method does reduce the amount of pyridine, but this method requires the assistance of microwaves, so it is not feasible for industrial scale-up
And even if a small amount of pyridine is used, due to the strong irritant of pyridine, it will cause greater damage to the health of the operator.
[0010] The method reported in the patent CN102875621 prepares diosmin by mixing and heating hesperidin, elemental iodine, inorganic alkaline reagents and organic solvents to 80-100°C. This method completely avoids the use of pyridine, and the production environment is greatly improved. But because aftertreatment adopts conventional alkali-dissolving acid analysis method equally, product purity is only about 95%, and the mixed solvent used is also unfavorable for the recycling of solvent, and because the disproportionation reaction of inorganic alkali and iodine in the reaction causes iodine to be difficult to reclaim, Thereby increasing production cost, this has also limited the application of this invention on mass production

Method used

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  • A kind of preparation method of diosmin
  • A kind of preparation method of diosmin
  • A kind of preparation method of diosmin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add 2kg of hesperidin and 0.92kg of iodine into a 20L reaction kettle, then add 8L of morpholine, start stirring and raise the temperature, wait until the temperature rises to 40°C and the sample is completely dissolved, keep it at 45°C±5°C for 0.5 hours, then raise the temperature to Insulate and stir at 70°C±5°C for 1.5-3 hours (the complete conversion of hesperidin monitored by HPLC is defined as the end point of the reaction). Recover the solvent until the reactant becomes viscous, add 12L of purified water, stir, stir well, pour the material into the reaction buffer tank, add hydrochloric acid to adjust the pH=5~7 to crystallize, filter to obtain filter cake and filtrate, add hydrochloric acid Adjust the pH of the filtrate to 2, slowly add 0.41 kg of 30% hydrogen peroxide, filter, and recover elemental iodine. The filter cake was washed with a large amount of water to obtain crude diosmin. Add 12L of purified water and 0.39kg of sodium hydroxide into the purificat...

Embodiment 2

[0029] Add 2kg of hesperidin and 0.92kg of iodine into a 20L reaction kettle, then add 10L of N-methylmorpholine, start stirring and raise the temperature. When the temperature rises to 40°C, the sample is completely dissolved, and keep it at 45°C±5°C for 0.5 hours. Then raise the temperature to 80° C.±5° C. and keep stirring for 1.5 to 3 hours (the complete conversion of hesperidin monitored by HPLC is defined as the end point of the reaction). Recover the solvent until the reactant becomes viscous, add 12L of purified water, stir well, pour the material into the reaction buffer tank, add hydrochloric acid to adjust the pH=5~7 for crystallization, filter to obtain filter cake and filtrate, add hydrochloric acid to adjust the filtrate pH = 2, slowly add 0.41 kg of 30% hydrogen peroxide, filter to recover elemental iodine. The filter cake was washed with a large amount of water to obtain crude diosmin. Add 12L of purified water and 0.39kg of sodium hydroxide into the purificat...

Embodiment 3

[0031]Add 2kg of hesperidin and 0.92kg of iodine into a 20L reaction kettle, then add 12L of N,N-diisopropylethylamine, start stirring and raise the temperature, until the temperature rises to 40°C, the sample is completely dissolved, at 45°C±5°C Keep warm for 0.5 hours, then increase the temperature to 80°C±5°C and keep stirring for 1.5 to 3 hours (the complete conversion of hesperidin monitored by HPLC is defined as the end point of the reaction). Recover the solvent until the reactant becomes viscous, add 12L of purified water, stir well, pour the material into the reaction buffer tank, add hydrochloric acid to adjust the pH=5~7 for crystallization, filter to obtain filter cake and filtrate, add hydrochloric acid to adjust the filtrate pH = 2, slowly add 0.41 kg of 30% hydrogen peroxide, filter to recover elemental iodine. The filter cake was washed with a large amount of water to obtain crude diosmin. Add 12L of purified water and 0.39kg of sodium hydroxide into the purif...

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Abstract

The invention discloses a method for preparing green and economic diosmin. The method comprises three main steps of preparation, recycling and refining. Compared with a conventional method, the method thoroughly avoids use of pyridine and inorganic base, the production environment is greatly improved, the aftertreatment is simple, iodine and solvents can be recycled, the reaction conditions are gentle, the production cost is low, and meanwhile in the method, a crude product is not refined in a classic alkali solution acidification mode instead of a mode that diosmin is separated out, then the purity of a finished product can be up to 99%, the product quality can be improved, and moreover the method is simple and convenient to operate and applicable to industrial production.

Description

technical field [0001] The invention relates to a preparation method of medicine, in particular to a preparation method of diosmin. Background technique [0002] Diosmin, the chemical name is 7-{[6-O-(6-deoxy-α-L-mannose)-β-D-glucopyranose]oxyl}-5-hydroxy-2-(3- Hydroxy-4-methoxybenzene)-4H-L-benzopyran-4-one is a kind of grayish yellow or light yellow hygroscopic powder, dissolved in dimethyl sulfoxide and dilute sodium hydroxide solution, almost insoluble In ethanol (96%) and water, its structure is as follows: [0003] [0004] Diosmin has a vitamin P-like effect, can reduce vascular fragility and abnormal permeability, and can be used as an adjuvant treatment for the prevention and treatment of hypertension and arteriosclerosis. The effect of treating capillary fragility is stronger than that of rutin and hesperidin. And it has the characteristics of low toxicity. It can also reduce blood viscosity and enhance the flow rate of red blood cells, thereby reducing the s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H17/07C07H1/00C07H1/06C01B7/14
CPCY02P20/582
Inventor 童耀吴舰林峰徐丹朱春霞田舟山
Owner NANJING CHIA TAI TIANQING PHARMA
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