Diosmin producing process

A production method, the technology of diosmin, is applied in the direction of sugar derivatives and organic chemistry, which can solve the problems of long process route, complex reaction, and influence on reaction speed, and achieve simple process operation, high product purity, and reduced use Effect

Inactive Publication Date: 2007-12-19
SICHUAN XIELI PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] Method 1 has a long process route, complex reactions, difficult control of related impurities, low yield and process efficiency, and is difficult to industrialize
[0008] In the method two, solid alkali sodium carbonate is added in the reaction system, which has a strong impact on the reaction speed and the reaction purity, making it difficult to control the relevant impurities of the product
Deiodination with morpholine is costly and pollutes the environment

Method used

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  • Diosmin producing process

Examples

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Effect test

Embodiment 1

[0019] The method of this embodiment 1 is 100 grams of hesperidin, add 200 milliliters of dimethylformamide, then evaporate to dryness under reduced pressure, remove the crystal water in the hesperidin like this, then add 500 milliliters of pyridine, 4 grams of iodine, heat to reflux React for 12 hours, concentrate to dryness under reduced pressure, then add 100 ml of 5% sodium hydroxide aqueous solution, stir at 30 degrees for 8 hours, filter, adjust pH to 4 with dilute hydrochloric acid, filter the obtained solid, wash with water until neutral , dried to obtain 90 grams of light yellow solid powder-diosmin, product melting point, iodine residue, solvent residue, related impurities and content all up to standard.

Embodiment 2

[0021] Method 2 of this embodiment is to add 100 milliliters of hesperidin to 100 milliliters of dimethylformamide, then distill to dryness under reduced pressure, thus removing the crystal water in hesperidin, then add 800 milliliters of pyridine and 5 grams of iodine, and heat to reflux React for 8 hours, concentrate to dryness under reduced pressure, then add 200 ml of 2.5% sodium hydroxide, stir at 80 degrees for 2 hours, filter, adjust pH to 4.5 with dilute hydrochloric acid, filter the obtained solid, wash with water until neutral, Dry to obtain 93 grams of light yellow solid powder-diosmin, the product melting point, iodine residue, solvent residue, related impurities and content are all up to standard.

Embodiment 3

[0023] Method 3 of this embodiment is 100 grams of hesperidin, add 300 milliliters of dimethylformamide, then evaporate to dryness under reduced pressure, remove the crystal water in the hesperidin like this, then add 300 milliliters of pyridine, 4.5 grams of iodine, heat to reflux React for 16 hours, concentrate to dryness under reduced pressure, then add 100 ml of 5% sodium hydroxide, stir at 50°C for 6 hours, filter, adjust pH to 4.5 with dilute hydrochloric acid, filter the obtained solid, wash with water until neutral, Dry to obtain 85 grams of light yellow solid powder-diosmin, the product melting point, iodine residue, solvent residue, related impurities and content are all up to standard.

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Abstract

The Diosmin producing process includes the following steps: adding high boiling point solvent into hesperidin, vacuum self distillation to eliminate crystal water from hesperidin, adding reaction solvent in the amount of 3-20 times weight of hesperidin and iodine in 0.3-0.6 time to react at 80-120 deg.c for 8-20 hr, vacuum concentrating, adding water solution of alkali and hydrolyzing at 30-80 deg.c for 1-8 hr, regulating pH value with dilute acid solution to acidity, filtering to obtain solid, water washing to neutrality, and drying to obtain Diosmin product. The process has low cost, high product purity and environment friendship.

Description

Technical field: [0001] The present invention is related to the production method of diosmin (Diosmin also called diosmin). Background technique: [0002] Diosmin is a natural flavonoid venous affinity drug, which can quickly relieve the symptoms of acute hemorrhoids, relieve symptoms for patients with chronic hemorrhoids, prevent the recurrence of acute hemorrhoids, and significantly reduce post-hemorrhoidectomy. bleeding. It can also be used for chronic venous insufficiency, such as varicose veins, lower extremity ulcers, etc. [0003] Due to the very low content of diosmin in natural plants, the current medicinal diosmin is chemically synthesized from the naturally extracted drug hesperidin. [0004] The current general synthesis method of diosmin: [0005] Method 1: hesperidin—hesperidin protected by acetyl group—oxidation reaction of bromine water—hydrolysis—diosmin. [0006] Method 2: hesperidin - solid base to remove water - iodine substitution reaction - morpholi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/07
Inventor 张光跃张强
Owner SICHUAN XIELI PHARM CO LTD
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