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Preparation method of 11 alpha,17 alpha-dyhydroxyl-androst-4-ene-3,20-dione

A technology of dihydroxy and androster, which is applied in the field of 11α, can solve problems such as the inability to realize industrial production, and achieve the effect of increasing the conversion rate and increasing the concentration of substrate feeding

Active Publication Date: 2011-05-18
台州仙琚药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, the industrialized production of B prepared from A cannot be realized

Method used

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  • Preparation method of 11 alpha,17 alpha-dyhydroxyl-androst-4-ene-3,20-dione
  • Preparation method of 11 alpha,17 alpha-dyhydroxyl-androst-4-ene-3,20-dione
  • Preparation method of 11 alpha,17 alpha-dyhydroxyl-androst-4-ene-3,20-dione

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] 1000ml of medium was contained in a 2-liter flask, and the medium included 2% (weight percent) glucose, 2.2% (weight percent) corn steep liquor, 0.11% (weight percent) (NH 4 ) 2 SO 4 ; Sterilize the medium at 120°C for 30 minutes in an autoclave; cool down, and then inoculate the slant culture of Ochraus strains in the medium; inoculate the medium inoculated with the strain at 30±1°C in a shaker Cultivate for 24 hours at 165rpm;

[0063] After such precultivation, inoculate again in the 20 liters fermentor that is covered with 19 liters and the aseptic medium of precultivation final composition identical as above-mentioned; Add 1.0ml foam enemy additionally to reduce foaming;

[0064] After a 12-hour growth period at an overpressure of 0.4-0.6 bar and a temperature of 30±1°C, aerate at 4 liters / min and stir at 165 rpm;

[0065] Add 150g of 17α-hydroxy-androst-4-ene-3,20-dione (intermediate A) to 600ml of ethanol to dissolve, then put it into the culture medium; conti...

Embodiment 2

[0069] 1000ml of culture medium was housed in a 2-liter flask, and the culture medium included 2% (weight percent) glucose, 2% (weight percent) corn steep liquor, 0.10% (weight percent) (NH 4 ) 2 SO 4 ; Sterilize the medium at 120°C for 30 minutes in an autoclave; cool down, then inoculate the slant culture of Metarhizium anisopliae strains in the medium; inoculate the medium inoculated with the strain at 28±1°C in a shaker Cultivate at 165rpm for 24 hours;

[0070] After such precultivation, inoculate again in the 20 liters fermentor that is covered with 19 liters and the aseptic medium of precultivation final composition identical as above-mentioned; Add 1.0ml foam enemy additionally to reduce foaming;

[0071] After a 12-hour growth period at an overpressure of 0.4-0.6 bar and a temperature of 28±1°C, aerate at 4 liters / min and stir at 165 rpm;

[0072] Add 200g of 17α-hydroxy-androst-4-ene-3,20-dione (intermediate A) to 600ml dimethylformamide (DMF) to dissolve, then pu...

Embodiment 3

[0076] 1000ml of medium was housed in a 2-liter flask, and the medium included 3% (weight percent) glucose, 3% (weight percent) corn steep liquor, 0.13% (weight percent) (NH 4 ) 2 SO 4 ; Sterilize the medium at 120°C for 30 minutes in an autoclave; cool down, then inoculate the slant culture of Rhizopus niger strain in the medium; inoculate the medium inoculated with the strain at 26±1°C in a shaker Cultivate at 165rpm for 24 hours;

[0077] After such precultivation, inoculate again in the 20 liters fermentor that is covered with 19 liters and the aseptic medium of precultivation final composition identical as above-mentioned; Add 1.0ml foam enemy additionally to reduce foaming;

[0078] After a 12-hour growth period at an overpressure of 0.4-0.6 bar and a temperature of 26±1°C, aerate at 4 liters / min and stir at 165 rpm;

[0079] Add 100g of 17α-hydroxy-androst-4-ene-3,20-dione (intermediate A) into 600ml of methanol to dissolve, and then put it into the culture medium; c...

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Abstract

The invention discloses a preparation method of 11 alpha,17 alpha-dihydroxyl-androst-4-ene-3,20-dione. In the method, microorganisms are utilized to convert 17 alpha-hydroxyl-androst-4-ene-3,20-dione into 11 alpha,17 alpha-dihydroxyl-androst-4-ene-3,20-dione. The method comprises the following steps: 1) preparing and treating a culture medium; 2) feeding; 3) extracting mycelia; and 4) refining. In the method provided by the invention, microorganism fermentation is adopted, thus the conversion rate and the substrate feeding concentration are greatly increased, and the large-scale industrialized production of the steroid intermediate 11 alpha,17 alpha-dyhydroxyl-androst-4-ene-3,20-dione is realized.

Description

technical field [0001] The invention relates to a steroid compound, in particular to a preparation method of 11α, 17α-dihydroxy-androst-4-ene-3,20-dione. Background technique [0002] 11α, 17α-dihydroxy-androst-4-ene-3,20-dione (intermediate B) is a very important intermediate in steroids, and it can be used as a raw material to prepare a variety of corticosteroids, especially In the field of steroid hormone production with phytosterol as the starting material in the future, it is an essential intermediate in the production process of various corticosteroids. These corticosteroids can treat a variety of human diseases, and are of great significance to the protection of people's health. [0003] The chemical formula of intermediate B is as follows: [0004] [0005] Intermediate B can be converted from 17α-hydroxy-androst-4-ene-3,20-dione (Intermediate A). The chemical formula of Intermediate A is as follows: [0006] [0007] The reaction formula for converting inte...

Claims

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Application Information

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IPC IPC(8): C12P15/00
Inventor 王建李龙应明华朱秀燕
Owner 台州仙琚药业有限公司
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