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Method for refining betamethasone

A betamethasone and refining method technology, applied in the direction of steroids, organic chemistry, etc., can solve the problems of low yield of betamethasone fine products, product quality can not meet the requirements, etc., achieve low cost, small risk, increase yield The effect of rate and quality

Inactive Publication Date: 2014-04-16
SHANGHAI NEW HUALIAN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the impurity requirements of betamethasone bulk drug are increased. The current method adopts ethyl acetate single solvent refining, and the yield of betamethasone refined product is as low as 85%, and the quality of the product does not meet the requirements, only 99.0%.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Drop into 20.0g betamethasone crude product in 500ml reaction bottle, be that the dichloromethane and the methanol mixed solvent of 1:1.8 are heated to 50 degree with 280ml volume ratio and carry out reflux dissolving clear, reflux 10 minutes, the temperature in the reaction bottle is reduced to 2 temperature to 5 degrees, began to slowly add 130ml of purified water dropwise, after the dropwise addition, continued to insulate and stir at 0 to 5 degrees for 40 minutes, let stand for 40 minutes, filtered, and the solid obtained by filtration was dried at a temperature of 80 degrees for 8 hours to obtain Betamethasone fine product 18.2g, yield 91.0%, HPLC content is 99.7%.

Embodiment 2

[0025] Drop into 20.0g betamethasone crude product in the 500ml reaction bottle, be that the dichloromethane and the ethanol mixed solvent of 1:1.6 are heated to 56 degree with 260ml volume ratio and carry out reflux dissolving clear, reflux 10 minutes, the temperature in the reaction bottle is reduced to 5 temperature to 8 degrees, began to slowly add 180ml of purified water dropwise, and after the dropwise addition, continued to insulate and stir at 5 degrees to 8 degrees for 30 minutes, let stand for 30 minutes, filtered, and the solid obtained by filtration was dried at a temperature of 80 degrees for 8 hours to obtain Betamethasone fine product 18.4g, yield 92.0%, HPLC content is 99.5%.

Embodiment 3

[0027] Drop into 20.0g betamethasone crude product in the 500ml reaction bottle, be that the volume ratio of 260ml is 1:1.6 chloroform and the mixed solvent of methanol and heat to 60 degree and carry out reflux dissolving clear, reflux 10 minutes, the temperature in the reaction bottle is reduced to 5 degree to 8 degrees, start to slowly add 150ml of purified water dropwise, after the dropwise addition, continue to keep stirring at 5 degrees to 8 degrees for 45 minutes, let it stand for 45 minutes, filter, and dry the filtered solid at a temperature of 80 degrees for 8 hours to obtain beta Measone fine product 18.4g, yield 92.0%, HPLC content 99.7%.

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Abstract

The invention discloses a method for refining betamethasone, and betamethasone crude product is purified by organic solvent and water for obtaining betamethasone refined product, wherein, the organic solvent is a mixed solvent of halogenated hydrocarbon and alcohol. The method provided by the invention has the advantages of simple operation and greatly improved product yield and quality. Double-solvent and water system can effectively control impurity removal, and the refined product content of the prepared betamethasone is increased from 99.0% to 99.5% or more, and the yield is increased from 85% to 90% or more; the refining method employs purified water, which has the advantages of little danger and low cost.

Description

technical field [0001] The invention belongs to the technical field of refining raw materials, and in particular relates to a method for refining betamethasone. Background technique [0002] Betamethasone is a high-efficiency corticosteroid drug, which can reduce the pathological changes of the body tissue to damaging stimuli, and has high curative effect, strong anti-inflammatory effect, and small side effects. It can treat serious diseases such as lupus erythematosus, rheumatoid arthritis, and asthma. It is widely used in domestic and international clinics. At present, the impurity requirements of betamethasone bulk drug are increased. The current method adopts ethyl acetate single solvent refining, and the yield of betamethasone refined product is as low as 85%, and the quality of the product does not meet the requirements, only 99.0%. . Contents of the invention [0003] In order to overcome the above-mentioned shortcomings and deficiencies in the prior art, the pres...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J5/00
Inventor 贺一君徐志超潘高峰卿文彬吴庆安周福群周秋火
Owner SHANGHAI NEW HUALIAN PHARMA
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