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Method for producing diosmin

A production method, the technology of diosmin, is applied in the direction of chemical instruments and methods, sugar derivatives, sugar derivatives, etc., which can solve the problems of operational risk, large volatilization loss, and high equipment requirements, and achieve low production cost and high yield. The effect of high rate and content, stable process

Inactive Publication Date: 2012-11-28
HUNAN YUANTONG PHARMA
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Problems solved by technology

Its disadvantage is that the refining of concentrated sulfuric acid requires high equipment, and the operation is dangerous; after heating, the volatilization loss is large, and the environment is seriously polluted.

Method used

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  • Method for producing diosmin
  • Method for producing diosmin
  • Method for producing diosmin

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Experimental program
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Embodiment Construction

[0024] The following production process should determine the cleanliness level of each area according to GMP specifications. The clean area is class 100,000.

[0025] First, the main reaction: put 360 kilograms of hesperidin, 42 kilograms of iodine and 1474 kilograms of pyridine (1500L) into the reaction kettle in sequence, close the kettle mouth, stir, slowly heat to reflux, stir and heat to a temperature of 110 ° C ± 5 under normal pressure ℃, keep the temperature at 110℃±5℃ and stir the reaction for 2 hours, then take a sample and detect it by HPLC detection method, stop the reaction when the concentration of hesperidin is less than 5% of diosmin, heat and recover the solvent pyridine;

[0026] Second, cleaning: Add 1 ton of pure water to the concentrated paste, add 79.5 kg of soda ash, stir for one hour, put the evenly stirred material into an open stainless steel mixing tank, add 150 kg of hydrochloric acid, and adjust the pH value to 7 , filter the material with a filte...

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Abstract

The invention discloses a method for producing diosmin. The method for producing the diosmin comprises the following production procedures of: performing a main reaction; cleaning; purifying; drying; grinding and mixing; and recovering iodine. According to the technical scheme, the conversion rate of an organic raw material hesperidin is over 95 percent; yield and content are high; the iodine, pyridine, methanol and ethanol can be recovered and reused on line and the recovery rate is 90 percent; material consumption and production cost are low; and the method has the advantages of simple technological process and stable process.

Description

technical field [0001] The invention relates to a method for producing diosmin. Background technique [0002] Diosmin, also known as diosmin, English name: Diosmin, molecular formula: C28H32O15, molecular weight: 608.54, chemical name: 3′,5,7-trihydroxy-4′-methoxyflavone; 7-{[6- O-(6-deoxy-α-L-mannose)-β-D-glucopyranose]oxy}-5-hydroxy-2-(3-hydroxy-4-methoxybenzene)-4H-L- Benzopyran-4-one. Diosmin is a kind of flavonoid drug, and its production is semi-synthesized from the hesperidin extracted from the natural Citrus aurantium fruit. [0003] According to statistics, the global annual consumption of diosmin is 3000t, mainly concentrated in Europe and South America. Since many other countries are also cultivating consumption habits of this drug, the demand is still growing and the prospect is promising. At present, my country is the main producer of hesperidin, with an annual output of several thousand tons, 90% of which are for export. The international production of dio...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H17/07C07H1/00
Inventor 金海霞杨向农赵劲松王平
Owner HUNAN YUANTONG PHARMA
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