Preparation method of carbazochrome sodium sulfonate

A technology of sodium carbosulfonate and sodium bisulfite, which is applied in the field of preparation of sodium carbosulfonate, can solve the problems of unsuitability for industrial production, complex operation, and many steps, and achieve good quality, short reaction steps, and mild reaction conditions Effect

Inactive Publication Date: 2012-10-31
JIANGSU HI STONE PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0023] Example 1:

[0024] A) Raw material dissolution reaction, put 50 parts of purified water, 10 parts of adrenaline color hydrazone, 8 parts of sodium bisulfite and 1 part of ascorbic acid weighed in parts by weight into the reaction tank, stir while heating, when the heating temperature is At 60°C, the solids are completely dissolved, and the reaction is kept at 60°C for 30 minutes to obtain a reaction liquid;

[0025] B) Decolorization and separation. Add a decolorizing agent, namely medicinal activated carbon, to the reaction solution obtained in step A. The added amount of medicinal activated carbon is 0.15% of the weight of the reaction solution. Stir and decolorize for 60 minutes at a temperature of 60°C, and the decolorization is complete Afterwards, spin filtration, wash the residue with purified water, spin dry, and combine the filtrates to obtain a liquid to be crystallized;

[0026] C) Crystallize, adjust the pH of the liquid to be crystallized from step B) to 5.5...

Example Embodiment

[0028] Example 2:

[0029] A) Raw material dissolution reaction, put 80 parts of purified water, 12 parts of adrenaline color hydrazone, 10 parts of sodium bisulfite and 5 parts of ascorbic acid weighed in parts by weight into the reaction tank, stir while heating, when the heating temperature is At 70°C, the solids are completely dissolved, and the reaction is kept at 70°C for 60 minutes to obtain a reaction liquid;

[0030] B) Decolorization and separation. Add a decolorizing agent, namely medicinal activated carbon, to the reaction liquid obtained in step A. The amount of medicinal activated carbon added is 0.16% of the weight of the reaction liquid. Stir and decolorize for 60 minutes at a temperature of 70°C, and the decolorization is complete Afterwards, spin filtration, wash the residue with purified water, spin dry, and combine the filtrates to obtain a liquid to be crystallized;

[0031] C) Crystallization, adjust the pH of the liquid to be crystallized from step B) to 6...

Example Embodiment

[0033] Example 3:

[0034] A) Raw material dissolution reaction, put 100 parts of purified water, 15 parts of adrenaline color hydrazone, 12 parts of sodium bisulfite and 3 parts of ascorbic acid weighed in parts by weight into the reaction tank, stir while heating, when the heating temperature is At 90°C, the solids are completely dissolved, and the reaction is kept at 90°C for 20 minutes to obtain a reaction liquid;

[0035] B) Decolorization and separation. Add a decolorizing agent, namely medicinal activated carbon, to the reaction liquid obtained in step A). ​​The amount of medicinal activated carbon added is 0.155% of the weight of the reaction liquid. Stir and decolorize for 40 minutes at a temperature of 90°C. The decolorization is complete Afterwards, spin filtration, wash the residue with purified water, spin dry, and combine the filtrates to obtain a liquid to be crystallized;

[0036] C) Crystallization, adjust the pH of the liquid to be crystallized from step B) to ...

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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 ...

Claims

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Application Information

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IPC IPC(8): C07D209/30
Inventor 王多平姚宇
Owner JIANGSU HI STONE PHARMA
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