Preparation method of cortisone acetate

A technology for cortisone acetate and epihydrocortisone, applied in the field of steroid drug preparation, can solve problems such as unfavorable applications, and achieve the effects of simplifying production operations, reducing production costs, and reducing reaction impurities

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

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Problems solved by technology

These limiting factors are not conducive to the application of TEMPO catalytic oxidation in the industrial production of steroids

Method used

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  • Preparation method of cortisone acetate

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Experimental program
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Embodiment 1

[0025] Acetylation reaction: Add 20 g of epihydrocortisone, 5.6 g of barium acetate, and 120 ml of glacial acetic acid to the reaction bottle in sequence, and stir at 20° C. for 0.5 hour. Then the temperature was lowered to 15°C, and 14ml of acetic anhydride was added dropwise. After the dropwise addition was completed, the reaction was maintained at 25° C. to 30° C. for 8 hours.

[0026] Oxidation reaction: Cool down the acetylation reaction solution after the above heat preservation reaction to 10°C, add dropwise a solution of 0.8g sodium bromide dissolved in 80ml sodium hypochlorite solution with a sodium hypochlorite content ≥ 8.0% in terms of available chlorine. After the addition is complete, keep the reaction at 13°C to 15°C for 3 hours. Slowly add the reaction solution into 1600ml of ice water pre-cooled to 0°C-5°C. After the addition is complete, continue to stir at 0°C-5°C for 0.5 hour, filter with suction, wash with water, and drain to obtain crude cortisone acetat...

Embodiment 2

[0028] Acetylation reaction: Add 20 g of epihydrocortisone, 3.6 g of barium acetate, and 80 ml of glacial acetic acid to the reaction bottle in sequence, and stir at 20° C. for 0.5 hour. Then the temperature was lowered to 15°C, and 40ml of acetic anhydride was added dropwise. After the dropwise addition was completed, the reaction was maintained at 25° C. to 30° C. for 6 hours.

[0029] Oxidation reaction: Cool down the acetylation reaction solution after the above heat preservation reaction to 10°C, add dropwise a solution of 0.4g sodium bromide dissolved in 40ml sodium hypochlorite solution with a sodium hypochlorite content ≥ 8.0% in terms of available chlorine. After the addition is complete, keep the reaction at 13°C to 15°C for 4 hours. Slowly add the reaction solution into 1600ml of ice water pre-cooled to 0°C-5°C. After the addition is complete, continue to stir at 0°C-5°C for 0.5 hour, filter with suction, wash with water, and drain to obtain crude cortisone acetate...

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Abstract

The invention discloses a preparation method of cortisone acetate. According to the method, hydrocortisone is taken as an initiator, and preparation is performed through steps including acetylation, oxidization and the like. Sodium hypochlorite which is low in cost and environment-friendly is used for replacing chromic anhydride which is high in cost and larger in toxicity and serves as an oxidizing agent in an oxidation reaction, and a catalyst which cannot be recovered and recycled is not required in an oxidation reaction process. The preparation method of the cortisone acetate has the advantages that the production cost is reduced, the production operation is simplified, environmentally hazardous chromium ion wastewater is not discharged, and the method is suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of steroid medicine preparation, in particular to a preparation method of cortisone acetate. Background technique [0002] Cortisone acetate is an adrenal cortex hormone drug, which is mainly used to treat primary or secondary adrenal insufficiency, and can reduce the pathological response of body tissues to damaging stimuli. Cortisone acetate can also be used as an important intermediate for the production of steroid drugs such as hydrocortisone and methylprednisolone, and the market prospect is very broad. [0003] The preparation process of cortisone acetate is introduced in "National Compilation of Raw Materials Processes" (State Administration of Medicine, 1980). One of the preparation processes uses epihydrocortisone as a starting material, and undergoes esterification and oxidation to obtain cortisone acetate. The mass total yield of epihydrocortisone in this process is 70%. Hydrocortisone is a by-p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J5/00
Inventor 廖俊曾建华汤鑫欣仇玲玲喻致蓉刘小波李桂莲魏旭力薛俊冯旋
Owner HUAZHONG PHARMA
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