Preparation method of etamsylate

Abstract

The invention relates to a preparation method of etamsylate. The etamsylate is prepared by virtue of three steps, namely sulfonating, salifying and refining, and the entire preparation process is free from an organic solvent, so that cost and pollution are reduced; in addition, a crude product is refined by virtue of absolute ethyl alcohol which serves as a solvent; therefore, the entire process is not only lower in cost but also more environment-friendly; the etamsylate prepared by the method is relatively higher in mass percentage; in conclusion, the preparation method disclosed by the invention has the advantages of being simple in design, low in cost, environment-friendly and high in mass percentage.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a kind of phensulfame, in particular to a preparation method of phensulfame. Background technique [0002] Ethylamine phensulfate (CAS: 2624-44-4) is also known as hemostasis, and its chemical name is 2,5-dihydroxybenzenesulfonic acid diethylamine [0003] Salt, the structural formula is: , Pharmacokinetic studies have shown that fensulfame can increase the number of platelets, enhance the aggregation and adhesion of platelets, and promote the release of coagulation active substances, thereby producing a hemostatic effect. The effect is rapid, and the effect is the strongest 1 hour after intravenous injection. Generally, it can be maintained for 4 to 6 hours. This product is suitable for the prevention and treatment of surgical bleeding, thrombocytopenic purpura or allergic purpura and bleeding caused by other reasons, such as cerebral hemorrhage, gastroin...

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Problems solved by technology

[0003] Salt, the structural formula is: , Pharmacokinetic studies have shown that fensulfame can increase the number of platelets, enhance the aggregation and adhesion of platelets, and promote the release of coagulation active substances, thereby producing a hemostatic effect. The effect is rapid, and the effect is the strongest 1 hour after intravenous injection. Generally, it can be maintained for 4 to 6 hours. This product is suitable for the prevention and treatment of surgical bleeding, thrombocytopenic purpura or allergic purpura and bleeding caused by other reasons, such as cerebral hemorrhage, gastrointestinal bleeding, urinary tract bleeding, fundus hemorrhage, Gingival bleeding, epistaxis, etc., can be used together with other hemostatic drugs such as aminomethylbenzoic acid and vitamin K. This product has low toxicity. Among them, the benzoquinone method is to pass sulfur dioxide into the solution of diethylamine, ethanol and water to first prepare diethylamine sulfite, then add p-benzoquinone to the diethylamine sulfite solution at low temperature, and the reaction will reduce Ethanol is recovered by pressure distillation, and the crude product is precipitated after cooling. Add sodium bisulfite and activated carbon to decolorize water or dilute ethanol, and refine the product. The disadvantage of this process is: due to the incomplete reaction of p-benzoquinone, and the addition of phensulfame in the The high solubility in water and ethanol makes the product yield low, generally not more than 40%, and the price of p-benzoquinone is relatively high, and there are problems such as the absorption of tail gas when using sulfur dioxide. In addition, chlorosulfonic acid is used as sulfonation in the market. Before sulfonation, make hydroquinone and organic solvent azeotropic dehydration to anhydrous, but this method uses organic solvents, which pollutes the environment, and the hydrogen chloride gas generated during the sulfonation reaction pollutes the environment

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