Preparation method of prednisone

A technology of prednisone and hydrocortisone acetate, applied in the direction of microorganism-based methods, biochemical equipment and methods, steroids, etc., can solve the problems that are not suitable for industrial production, difficult to treat cyanide-containing wastewater, and potential safety hazards, etc. problems, to achieve the effect of being conducive to safe production, low operating cost and easy operation

Active Publication Date: 2020-10-16
ZHEJIANG SHENZHOU PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The synthesis method has long steps, and highly toxic cyanide reagent is used in the cyano group substitution reaction. The cyanide-containing wastewater is difficult to handle and has major safety hazards, and is not suitable for industrial production.

Method used

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  • Preparation method of prednisone
  • Preparation method of prednisone

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] A kind of preparation method of embodiment 1 prednisone, comprises the steps:

[0030] 1) Oxidation reaction: join 20g hydrocortisone acetate (1) in 300ml dichloromethane, add 200ml50% acetic acid aqueous solution, 10g manganese sulfate, 4ml70% chromium trioxide aqueous solution, control temperature 0 ℃ and stir reaction, after reaction finishes , adding 20ml of 20% aqueous sodium bisulfite solution, washing with water until neutral, concentrating, water analysis, filtering, and drying to obtain 18.9g of intermediate 2;

[0031] 2) Dehydrogenation reaction: 18.9 g of intermediate (2) obtained in step 1) was passed through the traditional Arthrobacter Simplex By-2-13 fermentation method to obtain 17.0 g of intermediate 3;

[0032] 3) Hydrolysis reaction: Add the 17.0 intermediate (3) obtained in step 2) into a mixed solvent of 85ml of dichloromethane and 85ml of methanol, add 17ml of 10% triethylamine aqueous solution, and control the temperature at 30°C to stir the reac...

Embodiment 2

[0033] A kind of preparation method of embodiment 2 prednisone, comprises the steps:

[0034] 1) Oxidation reaction: 20g hydrocortisone acetate (1) joins in 150ml dichloroethane, adds 100ml60% acetic acid aqueous solution, 5g manganese sulfate, 20ml 30% chromium trioxide aqueous solution, controls temperature 15 ℃ and stirs reaction, and reaction finishes Afterwards, 10ml of 30% potassium sulfite aqueous solution was added, washed with water until neutral, concentrated, water separated, filtered, and dried to obtain 18.8g of intermediate 2;

[0035] 2) Dehydrogenation reaction: 18.8g of intermediate (2) obtained in step 1) was passed through the traditional Arthrobacter Simplex By-2-13 fermentation method to obtain 16.8g of intermediate 3;

[0036] 3) Hydrolysis reaction: the 16.8 intermediate (3) obtained in step 2) is added to a mixed solvent of 160ml of chloroform and 100ml of isopropanol, 80ml of 1% aqueous sodium hydroxide solution is added, and the temperature is control...

Embodiment 3

[0037] A kind of preparation method of embodiment 3 prednisone, comprises the steps:

[0038] 1) Oxidation reaction: 20g hydrocortisone acetate (1) joins in 60ml chloroform, adds 60ml90% acetic acid aqueous solution, 2g manganese chloride, 10ml50% chromium trioxide aqueous solution, controls temperature 30 ℃ and stirs reaction, after reaction finishes , adding 4ml of 50% sodium sulfite aqueous solution, washing with water until neutral, concentrating, water analysis, filtering and drying to obtain 19.2g of intermediate 2;

[0039] 2) Dehydrogenation reaction: 19.2 g of intermediate (2) obtained in step 1) was passed through the traditional Arthrobacter Simplex By-2-13 fermentation method to obtain 17.0 g of intermediate 3;

[0040] 3) Hydrolysis reaction: Add the 17.0 intermediate (3) obtained in step 2) into 680ml of ethanol, add 34ml of 5% potassium carbonate aqueous solution, and control the temperature at 15°C to stir the reaction. After the reaction, add 35% acetic acid a...

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Abstract

The invention discloses a preparation method of prednisone, and belongs to the technical field of preparation and processing of medicines. According to the method, hydrocortisone acetate is used as aninitial raw material, and the prednisone is prepared through three steps of oxidation, biological fermentation dehydrogenation and hydrolysis. According to the preparation method of prednisone, the defects of a traditional process are overcome, the target product is high in purity, good in quality stability, high in yield, low in production cost and mild in reaction condition, a highly toxic cyanide reagent is prevented from being used, and the method is easy and convenient to operate, suitable for industrial production and wide in market prospect.

Description

technical field [0001] The invention relates to the technical field of preparation and processing of medicines, in particular to a preparation method of prednisone. Background technique [0002] Prednisone, the English name is Prednisone, the chemical name is 17α,21-dihydroxy-1,4-pregnadiene-3,11,20-trione. Prednisone has anti-inflammatory and anti-allergic effects, can inhibit the proliferation of connective tissue, reduce the permeability of capillary walls and cell membranes, reduce inflammatory exudation, and inhibit the formation and release of histamine and other toxic substances. It can promote the decomposition of protein into sugar and reduce the utilization of glucose. When used in conjunction with a large number of antimicrobials in severe toxic infections, it can have good cooling, anti-drug, anti-inflammatory, anti-shock and symptom relief effects. It has strong anti-inflammatory and anti-allergic effects, less side effects, and is widely used in the market. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J5/00C12P33/02C12R1/06
CPCC07J5/0053C12P33/02
Inventor 邵振平王荣王炳乾王洪福黄橙橙雷灵芝王友富
Owner ZHEJIANG SHENZHOU PHARMA
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