Low-cost preparation method of diosmin

A low-cost technology of diosmin, applied in the field of drug preparation, can solve the problems of high cost and excessive iodine, and achieve the effect of reducing the amount of iodine and reducing costs

Pending Publication Date: 2021-08-24
HUNAN YUANTONG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] This method uses mo

Method used

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  • Low-cost preparation method of diosmin

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Effect test

Embodiment 1

[0024] A kind of low-cost preparation method of diosmin, the low-cost preparation method of described diosmin comprises the steps:

[0025] Put 600 liters of pyridine into the reactor, put 120 kilograms of hesperidin into it, stir and dissolve, then drop into 5 kilograms of iodine, heat the reaction, and start to feed ozone after the temperature reaches 90 degrees. Lasts 3 hours. Subsequently, samples were continuously taken to detect the reaction results, and the reaction was stopped when the content of hesperidin was less than 5%.

[0026] Continue heating to steam the pyridine in the reaction kettle and recycle until the material in the kettle becomes a paste, add pure water to disperse the reactant, and release the material after stirring evenly.

[0027] The material is adjusted to a neutral pH with hydrochloric acid, put into a box filter, and filtered to obtain the first filtrate, which is washed with pure water until the effluent is colorless.

[0028] Put the first ...

Embodiment 2

[0031] Drop into 720 liters of pyridine in the reaction kettle, 120 kilograms of hesperidin are dropped into, stir and dissolve, then drop into 8.6 kilograms of iodine, heat reaction, start to pass into ozone after the temperature reaches 95 degrees, the total amount of ozone passing into is 8.6 kilograms, passing into Lasts 3 hours. Subsequently, the reaction result was continuously sampled and detected, and the reaction was stopped when the content of hesperidin was less than 5%.

[0032] Continue heating to steam the pyridine in the reaction kettle and recycle until the material in the kettle becomes a paste, add pure water to disperse the reactant, and release the material after stirring evenly.

[0033] The material is adjusted to a neutral pH with hydrochloric acid, put into a box filter, and filtered to obtain the first filtrate, which is washed with pure water until the effluent is colorless.

[0034] Put the first filtrate into the tank, add sodium hydroxide solution...

Embodiment 3

[0037] Drop into 900 liters of pyridine in the reactor, drop 180 kilograms of hesperidin, stir and dissolve, then drop into 5 kilograms of iodine, heat reaction, start to pass into ozone after the temperature reaches 90 degrees, the total amount of ozone is 15 kilograms, pass into Lasts 2.5 hours. Subsequently, samples were continuously taken to detect the reaction results, and the reaction was stopped when the content of hesperidin was less than 5%.

[0038] Continue heating to steam the pyridine in the reaction kettle and recycle until the material in the kettle becomes a paste, add pure water to disperse the reactant, and release the material after stirring evenly.

[0039] The material is adjusted to a neutral pH with hydrochloric acid, put into a box filter, and filtered to obtain the first filtrate, which is washed with pure water until the effluent is colorless.

[0040] Put the first filtrate into the tank, add sodium hydroxide solution to dissolve, put filter paper i...

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Abstract

The invention discloses a low-cost preparation method of diosmin. The low-cost preparation method of diosmin comprises the following steps: dissolving hesperidin and iodine in pyridine; performing heating and introducing ozone until the concentration of hesperidin is lower than 5%; adjusting the pH value to be neutral, and performing filtering to obtain a first filtered substance; washing the first filtered substance with deionized water, adding alkali for dissolving, and performing filtering to obtain filtrate; and acidizing and recrystallizing the filtrate to obtain diosmin. The method has the effects of reducing the dosage of iodine and lowering the cost.

Description

technical field [0001] The invention relates to medicine preparation, in particular to a preparation method of diosmin. Background technique [0002] Diosmin is generally used for the treatment of hemorrhoid attacks. It is usually obtained by dehydrogenating the plant extract hesperidin. The common process is pyridine as a solvent, adding hesperidin and iodine for dehydrogenation reaction. After the reaction, the solvent is recovered and the product is Add water to precipitate, filter and wash to obtain the crude product, then dissolve it with alkali and filter to remove impurities, adjust the pH value to neutral with acid, filter, wash and dry to obtain the finished product. [0003] This method uses more iodine and is expensive. Contents of the invention [0004] In view of the above-mentioned deficiencies existing at present, the present invention provides a low-cost preparation method of diosmin, which can achieve the effects of reducing the amount of iodine and reduc...

Claims

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Application Information

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IPC IPC(8): C07H17/07C07H1/00
CPCC07H17/07C07H1/00
Inventor 金海霞赵劲松
Owner HUNAN YUANTONG PHARMA
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