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Preparation method of etamsylate

A technology of sulfoethylamine and hydroquinone, which is applied in the preparation of sulfonate, the preparation of organic compounds, the preparation of amino compounds, etc., can solve the problems of incomplete reaction of p-benzoquinone, high solubility, low toxicity, etc. The effect of protecting environmental quality scores, reducing costs and pollution, and designing simple

Inactive Publication Date: 2015-03-25
HENAN LINGXIAN SCI & TECHN PHARMA
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  • Abstract
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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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  • Preparation method of etamsylate

Examples

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Effect test

Embodiment 1

[0018] A kind of preparation method of phensulfame, it is characterized in that, it comprises the steps:

[0019] Step 1: Sulfonation: Add 50g of hydroquinone and 48g of concentrated sulfuric acid into the same three-necked bottle respectively, then heat in a water bath, and slowly raise the temperature until the hydroquinone is completely melted into a liquid state, and then stir the solution. , keep the three-necked bottle warm for 1 hour, after one hour keep the temperature down to 40°C, then add 100g of distilled water and 2g of activated carbon in turn to raise the temperature to 55°C, decolorize and stir for 30min, then filter to get 2,5-dihydroxy Benzenesulfonic acid solution;

[0020] Step 2: Salt formation: Pour the filtrate obtained in step 1 into another three-necked flask, cool the filtrate to 25°C, and then slowly add 2,5-dihydroxybenzenesulfonic acid to diethylamine in a mass ratio of 2 : the diethylamine of 1, after reaction finishes, cooling crystallization, t...

Embodiment 2

[0024] A kind of preparation method of phensulfame, it is characterized in that, it comprises the steps:

[0025] Step 1: Sulfonation: Add 60g of hydroquinone and 60g of concentrated sulfuric acid into the same three-necked bottle respectively, then heat in a water bath, and slowly raise the temperature until the hydroquinone is completely melted into a liquid state, and then stir the solution. , keep the three-neck flask warm for 1 hour, and then lower the temperature to 40°C after one hour of heat preservation, then add 120g of distilled water and 2.4g of activated carbon in turn to raise the temperature to 55°C, decolorize and stir for 30min, then filter to obtain 2,5-di Hydroxybenzenesulfonic acid solution;

[0026] Step 2: Salt formation: Pour the filtrate obtained in step 1 into another three-necked flask, cool the filtrate to 25°C, and then slowly add 2,5-dihydroxybenzenesulfonic acid to diethylamine in a mass ratio of 1 : the diethylamine of 1, after reaction finishes...

Embodiment 3

[0030] A kind of preparation method of phensulfame, it is characterized in that, it comprises the steps:

[0031] Step 1: Sulfonation: Add 80g of hydroquinone and 70g of concentrated sulfuric acid into the same three-necked bottle respectively, then heat in a water bath, and slowly raise the temperature until the hydroquinone is completely melted into a liquid state, then stir the solution, after stirring , keep the three-necked bottle warm for 1 hour, after keeping warm for one hour, lower the temperature to 40°C, then add 160g of distilled water and 3.2g of activated carbon in turn to raise the temperature to 55°C, decolorize and stir for 30min, then filter to obtain 2,5-di Hydroxybenzenesulfonic acid solution;

[0032] Step 2: Salt formation: Pour the filtrate obtained in step 1 into another three-necked flask, cool the filtrate to 25°C, and then slowly add 2,5-dihydroxybenzenesulfonic acid to diethylamine in a mass ratio of 2 : the diethylamine of 1, after reaction finish...

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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...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C309/42C07C211/05C07C303/32C07C303/44C07C209/00C07C209/84
Inventor 贺国超刘裕东郭有钢刘占领
Owner HENAN LINGXIAN SCI & TECHN PHARMA
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