The preparation method of palmatine

Abstract

The invention discloses a preparation method of fibrauretin which is applied in the chemical synthesis field of broad-spectrum antibiotics. The preparation method comprises the following steps: adding berberine hydrochloride in an organic solvent, and reacting at 100-150 DEG C under the catalysis of a Lewis acid to remove methylene and obtain an intermediate 2,3,9,10-tetrahydroxyberberine; placing the intermediate 2,3,9,10-tetrahydroxyberberine in a basic solvent to react under the action of a methylating agent at 30-40 DEG C and obtain an intermediate fibrauretin base; and heating the intermediate fibrauretin base in distilled water to dissolve, and adding hydrochloric acid to form the salt and obtain fibrauretin, wherein the organic solvent is selected from one of toluene and xylene, the Lewis acid is selected from one of aluminium chloride, boron tribromide and zinc chloride, and the methylating agent is dimethyl sulfate. The chemical synthesis method is adopted to prepare fibrauretin, thus the plant resource can be saved and the ecological environment can be protected; and berberine hydrochloride is used as the raw material, the raw material is cheap and easily available, the reaction steps of the synthetic route are short and the operations are simple, thus the cost can be saved and the method is suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation method of palmatine in the field of chemical synthesis of broad-spectrum antibacterial drugs. Background technique [0002] Palmatine, also known as palmatine, palmatine, palmitine, and palmatine, is an alkaloid (palmitine) extracted from Rhubarb vine, which belongs to heat-clearing and detoxifying drugs. Palmatine has a broad-spectrum antibacterial and antiviral effect, which can significantly promote the phagocytosis of bacteria by white blood cells, anti-inflammatory and enhance the body's immunity. It is generally used to treat gynecological inflammation, bacillary dysentery, enteritis, respiratory tract and urinary tract infection, surgical infection, conjunctiva diseases such as inflammation. In addition, palmatine also has a protective effect on the myocardium, can enhance myocardial contractility, and has anti-arrhythmic effects. Due to its definite curative effect, palmatine was included in the "Chinese...

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Problems solved by technology

Among the patents related to the synthetic method of palmatine, CN1687064A "Synthetic preparation method of antibacterial and anti-inflammatory drug palmatine" patent, CN100526311C "Synthetic method of palmatine" patent, both of these methods have long reaction routes, complicated operations, and low yields. Low cost, high cost, large amount of three wastes, difficult to handle, and great environmental hazards; CN100999522B "Preparation Method of Palmatine" patent, although the synthesis route is short, but has the disadvantages of poor quality and low content, it is not suitable for industrial production

CN102040604A "a synthesis method of palmatine" patent, using aluminum trichloride and berberine hydrochloride to react in methanol, in the presence of a phase transfer catalyst and pyridine, the methylene group is removed to obtain the intermediate o-dihydroxy hydrochloride Berberine is methylated under alkaline conditions with dimethyl sulfate, and crystallized with 95% ethanol and hydrochloric acid to obtain palmetine. This method needs to be stirred for 10 hours under the environmental conditions above 90 ° C, which is time-consuming and labor-intensive; There are many kinds of reagents used in the preparation process, the product yield is low, less than 50%, the product purity is low, and the content is less than 95%

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