Production process method for cortisone crude product

A production process, cortisone technology, applied in the production process field of crude pine products, can solve the problems of low yield, achieve the effect of product yield and quality improvement, and good compatibility of the system

Active Publication Date: 2012-12-19
HENAN LIHUA PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The defect of this process is that the reaction process is a semi-dissolution method, and the oil is produced at high temperature, and the yield is low, only 70-75%.

Method used

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  • Production process method for cortisone crude product

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Throw in 600ml of methanol, 450ml of chloroform, add 100g of cortisone acetate, stir to dissolve, after the solution is clear, cool down to -2°C to 0°C, add 5g of potassium hydroxide to 100ml of methanol solution to make a catalyst, and control the temperature at 0±2°C, after adding the potassium hydroxide-methanol solution, start to stand still and count, react for 40 minutes, the temperature is 0±2°C, use glacial acetic acid to neutralize the system to neutral, concentrate under reduced pressure, cool down to 0-10°C, filter, After drying, 83 g of cortisone crude product was obtained, the yield was 83%, and the content determined by ultraviolet spectrophotometry was 97.9%.

Embodiment 2

[0015] Throw in 600ml of methanol, 450ml of chloroform, add 100g of cortisone acetate, stir to dissolve, after the solution is clear, cool down to -2°C to 0°C, add 6g of potassium hydroxide to 100ml of methanol solution to make a catalyst, and control the temperature at 0±2°C, after adding the potassium hydroxide-methanol solution, start to stand still and count, react for 40 minutes, the temperature is 0±2°C, use glacial acetic acid to neutralize the system to neutral, concentrate under reduced pressure, cool down to 0-10°C, filter, After drying, 84 g of cortisone crude product was obtained, the yield was 84%, and the content determined by ultraviolet spectrophotometry was 98.2%.

Embodiment 3

[0017] Throw in 600ml of methanol, 450ml of chloroform, add 100g of cortisone acetate, stir to dissolve, after the solution is clear, cool down to -2°C to 0°C, add 6g of potassium hydroxide to 100ml of methanol solution to make a catalyst, and control the temperature at 0±2°C, after adding the potassium hydroxide-methanol solution, start to stand still and count, react for 40 minutes, the temperature is 0±2°C, use glacial acetic acid to neutralize the system to neutral, concentrate under reduced pressure, cool down to 0-10°C, filter, Drying, cortisone crude product 83.5g, yield 83.5%, ultraviolet spectrophotometric determination content 98.1%.

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Abstract

The invention discloses a production process method for a cortisone crude product, and belongs to the field of chemical pharmacy. By using cortisone acetate as a raw material, the method comprises the following steps of: (a), adding the cortisone acetate into a mixed solvent of methanol and trichloromethane to stir and dissolve, and clearly dissolving a system and reducing the temperature to be 0-2 DEG C; and (b), adding potassium hydroxide-methanol solution into a mixture; controlling the temperature to be 0+ / -2 DEG C to react for 40 minutes, and neutralizing, condensing, temperature-reducing, filtering and drying to prepare the cortisone crude product. According to the method, methanol serving as a single solvent in the traditional preparation process is replaced by the mixed solvent of the methanol and the trichloromethane, so that the yield and the quality of the product can be obviously improved.

Description

technical field [0001] The invention relates to a production process of cortisone, in particular to a production process of crude cortisone, which belongs to the field of chemical pharmacy. Background technique [0002] Cortisone is an adrenocortical hormone drug, mainly used in the replacement therapy of adrenal hypofunction and hypopituitarism, and can also be used for allergic and inflammatory diseases. The traditional cortisone production process uses cortisone acetate As a raw material, use a single solvent methanol as a solvent, solid sodium hydroxide as a catalyst, and react at 20-26 ° C. After the reaction is completed, neutralize, concentrate and crystallize, cool down, filter, and dry to obtain cortisone crude product. The following formula is the traditional preparation The reactive formula of the method: [0003] [0004] The defect of this technique is that the reaction process is a semi-dissolution method dissolution reaction, and oil is produced at a high ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J5/00
Inventor 姬卫忠王泉泉李合兴孙传源
Owner HENAN LIHUA PHARMA
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