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Novel production technology of diosmin

A technology of diosmin and new technology, which is applied in the new technology field of diosin production, and can solve problems such as unstable product quality

Inactive Publication Date: 2013-12-11
陕西惠丰制药有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

According to the method provided in the literature, although diosmin can be synthesized, the yield is 60-80%; the quality of the product is also unstable

Method used

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  • Novel production technology of diosmin
  • Novel production technology of diosmin
  • Novel production technology of diosmin

Examples

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Embodiment Construction

[0016] In a 500Kg reactor, add 300.0kg DMF, slowly add 100.0kg hesperidin, then add iodine 1.0~5.0kg and bromine water 1.0~3.0kg, slowly heat to 90~120℃ under stirring, and react at this temperature for 12~ 16h. Take a sample to detect the content of diosmin. When the content of hesperidin is lower than 1.0%, the reaction is finished, filtered, and the filtrate is recovered at 80-95° C. under a vacuum of - (0.05-0.07) Mpa to obtain a paste Dianoside. Add 1200kg of purified water to the paste-like diosmin, stir well, heat to 40-70°C, keep warm for 30-60min, press filter, wash with water until the outflowing water is clear. The filter cake was dried in an oven until the water content was 8-15%, and 108kg of the crude product was obtained. Put the crude product into the reaction kettle, add 864kg, 648kg, and 432kg of 85% ethanol respectively, and then add 400kg of iodine-removing agent, and stir and reflux for 60, 40, and 30 minutes respectively. Press filtration, wash the fil...

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Abstract

The invention discloses a novel production technology of diosmin, which comprises the following steps that a dehydrogenation reaction is performed; a crude diosmin product is prepared, dried, and subjected to iodine residual removal; a solvent residual of diosmin is removed; a fine diosmin product is dried, and subjected to a diosmin micronization technology; and micronized diosmin meeting a requirement of EP8.0 (European Pharmacopoeia 8.0) is obtained. The novel production technology has the characteristic of sociometric sustainable development; no harmful effect is exerted on an environment in a production process; more importantly, the consumption of a dehydrogenation agent is reduced to be 2-5% of that of hesperidin in the production process, so that a raw material resource is used fully to the greatest extent; the solvent and iodine residuals are removed effectively; and development requirements of a resource-saving and environment-friendly society are met.

Description

technical field [0001] The invention relates to a new technology for producing diosmin. Background technique [0002] Dianoside, chemical name: 7[[6-oxo-(6-deoxy-α-L-mannopyranosyl)-β-D-glucopyranose-]oxy]-5-hydroxy-2- (3-Hydroxy-4-methoxyphenyl)-4hydro-chromen-4-one. It is grayish yellow or light yellow, hygroscopic powder. Almost insoluble in water, soluble in dimethyl sulfoxide, almost insoluble in ethanol, soluble in dilute alkaline solution. Dianotin was first developed and marketed by the French company Servier in 1987. Dianoside can enhance pulsation force, reduce capillary permeability and enhance resistance, enhance lymphatic contraction and lymphatic drainage speed, and has the effect of treating acute or acute Hemorrhoid attack, varicose veins, lower abdominal swelling, improve venous tension, regulate microcirculation, clinically used for hemorrhoids and limb venous return disorders. Micronized diosmin can significantly reduce the pain of lower extremities in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/07C07H1/08
Inventor 李玉山
Owner 陕西惠丰制药有限公司
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