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Methylprednisolone preparation method

A technology of methylprednisolone and inoculum volume, applied in the fields of steroids, fermentation, organic chemistry, etc., can solve the problems of difficult industrial production, cumbersome operation of bromination and debromination reaction, etc., and achieve the effect of simple circuit and high yield

Inactive Publication Date: 2018-03-27
TIANJIN JINYAO GRP
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The patent CN104561217A uses 17α-OH-4,9-diene-3,20-dione-21-acetate as the starting material, and undergoes etherification, methylation, hydrogenation, fermentative dehydrogenation, bromination and dehydrogenation in sequence Bromination reaction to produce methylprednisolone, but the operation of bromination and debromination reaction is cumbersome and not easy for industrialized production

Method used

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Embodiment 1

[0047] Invention Example 1 Biotransformation

Embodiment 1-1

[0049] In 1L of water, ferment substrate formula 1 compound 50g, fermentation medium components glucose 15g, sucrose 5g, sodium nitrate 5g, ammonium sulfate 2g, dipotassium hydrogen phosphate 2g, potassium dihydrogen phosphate 5g, bubble enemy 0.4g, pH is 6.0. For the secondary culture of Arthrobacter simplex, after 24 hours of primary seed culture, insert 10% of the inoculum into the secondary seed medium, and after 22 hours of secondary culture, insert 15% of the inoculum into the above fermentation medium ; After 24 hours of culturing the primary seeds of Ochraus ochratum, they were inserted into the above-mentioned fermentation medium according to the 18% inoculum amount. Use a 20L fermenter for conversion, liquid volume 50%, tank pressure 0.05MPa, air flow 30m 3 / hr, temperature 28°C, stirring speed 200rpm, conversion for 72 hours, sampling by TLC analysis, the substrate conversion was over 90%, the sample was extracted with ethyl acetate, and the upper layer was sent to...

Embodiment 1-2

[0052] In 1L of water, ferment substrate formula 1 compound 50g, fermentation medium components glucose 25g, sucrose 10g, sodium nitrate 10g, ammonium sulfate 3g, dipotassium hydrogen phosphate 3g, potassium dihydrogen phosphate 3g, foam enemy 0.4g, pH is 6.0. For the secondary culture of Arthrobacter simplex, after 24 hours of primary seed culture, insert 8% of the inoculum into the secondary seed medium, and after 22 hours of secondary culture, insert 10% of the inoculum into the above fermentation medium ; After 24 hours of culturing the primary seeds of Ochraus ochratum, they were inserted into the above-mentioned fermentation medium according to the 12% inoculum amount. Use a 20L fermenter for conversion, with a liquid volume of 50%, a tank pressure of 0.04MPa, and an air flow rate of 20m 3 / hr, temperature 28°C, stirring speed 200rpm, conversion for 72 hours, sampling by TLC analysis, the substrate conversion was over 90%, the sample was extracted with ethyl acetate, an...

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Abstract

The invention discloses a methylprednisolone preparation method, wherein a compound represented by a formula 1 is used as a starting material, and biotransformation, oxidation, esterification, reduction and hydrolysis are sequentially performed to obtain the methylprednisolone.

Description

technical field [0001] The invention relates to a preparation method of methylprednisolone, which belongs to the technical field of pharmacy. Background technique [0002] Methylprednisolone is a chemical raw material drug of glucocorticoids. Due to its powerful anti-inflammatory, immunosuppressive, anti-allergic, anti-shock and other pharmacological effects, it is widely used clinically in respiratory diseases, endocrine disorders, rheumatic diseases, collagen diseases, Blood diseases, skin diseases, allergic states, nervous system diseases, etc. Compared with prednisone, it has the characteristics of quick onset, strong anti-inflammatory effect, short half-life, mineralocorticoid-like effect and weak influence on adrenal cortex function, and has a good curative effect / price ratio. The newer alternative products represent the clinical direction of glucocorticoids. This drug has been included as a national essential drug and a national basic medical insurance drug, and has...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J5/00C12P33/00
CPCC07J5/0053C12P33/10
Inventor 王淑丽张杰赵春霞
Owner TIANJIN JINYAO GRP
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