Preparation method of carbazochrome sodium sulfonate

Abstract

The invention relates to a preparation method of carbazochrome sodium sulfonate, belonging to the technical field of preparation of vascular hemostatics. The method comprises the following steps: raw materials dissolution and reaction: putting purified water, carbazochrome, sodium bisulfite and ascorbic acid into a reaction tank, heating while stirring until the solid substances are completely dissolved, and continuing keeping the temperature to react, thereby obtaining a reaction solution; decolorization and separation: adding a decolorant into the reaction solution, keeping the temperature while stirring for decolorization, after finishing decolorization, carrying out centrifugal filtration, washing residues with purified water, carrying out centrifugal drying, and merging the centrifugal filtrates to obtain a solution to be crystallized; crystallization: regulating the pH value of the solution to be crystallized with an alkaline matter, freezing to cooling, and standing to precipitate crystals; and refinement: carrying out centrifugal filtration on the crystals, washing, carrying out centrifugal drying, and drying in a vacuum drying oven to obtain the carbazochrome sodium sulfonate. The invention has the advantages of accessible reaction raw material, short reaction steps, mild reaction conditions, high reaction yield (up to more than 90%), better reaction product quality and high purity (up to more than 99%), and is convenient and simple to operate.

Description

technical field [0001] The invention belongs to the technical field of preparation of vascular hemostatic drugs, in particular to a preparation method of sodium carbosulfonate. Background technique [0002] Sodium carbosulfonate was first developed by Japan Tanabe Pharmaceutical Co., Ltd., and has been included in the twelfth edition of the Japanese Pharmacopoeia (1992) by the Japanese Ministry of Health and Welfare. [0003] Sodium carbosulfonate can enhance the elasticity of capillaries, reduce the permeability of capillaries, promote the retraction of broken capillaries, stabilize the acidic mucopolysaccharides in capillaries and surrounding tissues, significantly shorten the bleeding time, and promote the activity of thrombin and The dissolution of fibrinogen, and then the formation of thrombus at the bleeding site to achieve hemostasis, is an effective hemostatic drug for various bleeding caused by increased capillary permeability and massive bleeding caused by various ...

AI Technical Summary

Problems solved by technology

The article "Revised Structure of the Adrenochrome Sulfonate, Ac-17 and Ac-44" published by Mitsutaka Kawazu et al. provides a method for synthesizing sodium carbosulfonate, which uses adrenaline as a raw material and undergoes cyclization under the action of silver oxide Generate adrenochrome, adrenochrome and semicarbazide are substituted to generate carbacol, and carbacol reacts with a weakly alkaline reducing agent to generate carbazone sodium. This synthesis method has many steps and more expensive reagents are used in the reaction. , the operation is also complicated, so it is not suitable for industrial production

[0005] A synthetic method provided by Zhu Baoquan et al. ("New Drug Synthesis Manual", pp. 181-184). Electrolytic oxidation produces adrenochrome, and then substitutes with semicarbazide to form carbacide, which reacts with a weakly alkaline reducing agent to generate carbacide sodium. The same synthesis method has more steps, and electrolytic oxidation is used in the reaction. Operation It is also more complicated, so it is also not suitable for industrial production