Preparation of diosmin by one-pot cooking method from hesperidin
A technology of diosmin and hesperidin, which is applied in the direction of organic chemistry and can solve the problem of low product yield
Inactive Publication Date: 2015-11-25
陕西惠丰制药有限公司
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Problems solved by technology
During the crude product preparation process, because the reaction concentrate contains a large amount of impurities, the product obtained by the alkali-dissolved acid precipitation method used to have a low yield and a reddish-brown color. Now, the precipitation method is used, which has a high yield, high content, and good color. The crude product is prepared The quality of the product is related to the yield of the product and the quality of the boutique
Method used
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Experimental program
Comparison scheme
Effect test
Embodiment Construction
[0011] Method 1: In a 500Kg reactor, add 300.0Kg of solvent A, slowly add 100.0kg of hesperidin, then add 1.0-3.0kg of excipients B, 3.0-4.5kg of excipients C and slowly heat to 90-100°C while stirring, React at this temperature for 5 to 16 hours. A sample is taken to detect the content of diosmin, and the reaction is stopped when the content of hesperidin is lower than 0.5%. Recover the solvent at a vacuum of -(0.01~0.07) Mpa, add 500~1000L of purified water to the residue, heat slightly, stir thoroughly to form a paste, and then filter to obtain a yellow filter cake, add purified water to the filter cake and stir Into a paste, precipitated, filtered to obtain a wet crude product of diosmin. Put the crude diosmin into a refining tank, add 500-800L of purified water, fully stir to form a paste, add 50-100L of 10% sodium hydroxide solution, fully stir to dissolve, add 1.5-2.5kg of activated carbon, and heat to 40-60°C Insulate for 30 minutes, filter, the filtrate is clear yel...
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Abstract
The invention discloses preparation of diosmetin from hesperidin by a using one-pot boiling method. The method comprises the following steps: reacting in one-pot boiling manner, preparing a crude product, preparing a refined product, drying, crushing, detecting, mixing and packaging. According to the method, two steps for two-step reactions are integrated into one step and are performed simultaneously, and moreover an automatic temperature controller is arranged on a reaction kettle, so that the situation that the temperature is raised or reduced through manual operation is avoided, and the production efficiency is greatly improved; particularly the dehydrogenation agent consumption is only 1-5% of that in the conventional method, so that the production cost is greatly lowered. The judgment on a final reaction point is controlled through high-efficiency liquid phase, so that the reaction precision is greatly improved; acid hydrolysis in the conventional method is avoided, the reaction conditions are mild, the reaction time is short, the yield and purity are both improved, resources is saved, and environmental friendliness is achieved.
Description
technical field [0001] The invention relates to the preparation of diosmin by one-pot cooking method of hesperidin Background technique [0002] Diosmetin is a flavonoid compound, yellow powder, molecular formula C 16 h 12 o 6 , molecular weight 300.26, melting point 256-258°C. Dioxynignin has anti-oxidative, anti-infective, anti-shock and anti-mutagenic and anti-allergic properties, and is widely used in functional foods, cosmetics and future medicines. It can inhibit the activity of human CYP1A enzyme and the carcinogenic activity of carcinogens. It can be used as an antiviral drug for the treatment of HIV and other viral infections, an inhibitor of MAP kinase, and can treat various inflammations. It can diuresis and lower blood pressure. effect. Diyerin can be extracted from the peel of lemon Citruslimon (L.) Burm. The production process mainly consists of ethanol extraction, concentrated extraction, column chromatography, crystallization and other processes, but the...
Claims
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IPC IPC(8): C07D311/30
CPCC07D311/30
Inventor 李玉山
Owner 陕西惠丰制药有限公司