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

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Problems solved by technology

Therefore, the industrialized production

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

Example Embodiment

[0061] Example 1:

[0062] A 2 liter flask is filled with 1000ml culture medium, which includes 2% (weight percentage) glucose, 2.2% (weight percentage) corn steep liquor, 0.11% (weight percentage) (NH 4 ) 2 SO 4 ; Sterilize the medium in an autoclave at 120°C for 30 minutes; cool, and then inoculate the slant culture of the Aspergillus ochrae strain in the medium; place the medium inoculated with the strain in a shaker at 30±1°C Incubate at 165rpm for 24 hours;

[0063] After such pre-cultivation, it is then inoculated into a 20-liter fermenter covered with 19 liters of sterile medium with the same final composition as the above-mentioned pre-cultivation; another 1.0 ml foam is added to reduce foaming;

[0064] After 12 hours of growth period at an overpressure of 0.4~0.6bar and a temperature of 30±1℃, aeration at 4L / min and stirring at 165rpm;

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

Example Embodiment

[0068] Example 2:

[0069] A 2 liter flask is filled with 1000 ml of culture medium, which includes 2% (weight percentage) glucose, 2% (weight percentage) corn steep liquor, 0.10% (weight percentage) (NH 4 ) 2 SO 4 ; Sterilize the medium in an autoclave at 120°C for 30 minutes; cool, then inoculate the slant culture of Metarhizium anisopliae strain in the medium; place the medium inoculated with the strain in a shaker at 28±1°C Cultivate for 24 hours at 165rpm;

[0070] After such pre-cultivation, it is then inoculated into a 20-liter fermenter covered with 19 liters of sterile medium with the same final composition as the above-mentioned pre-cultivation; another 1.0 ml foam is added 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, aeration at 4 liters / min and stirring at 165 rpm;

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

Example Embodiment

[0075] Example 3:

[0076] A 2 liter flask is filled with 1000ml of culture medium. The culture medium includes 3% (wt%) glucose, 3% (wt%) corn steep liquor, 0.13% (wt%) (NH 4 ) 2 SO 4 ; Sterilize the medium in an autoclave at 120°C for 30 minutes; cool, then inoculate the slant culture of the Rhizopus niger strain in the medium; place the medium inoculated with the strain in a shaker at 26±1°C Cultivate for 24 hours at 165rpm;

[0077] After such pre-cultivation, it is then inoculated into a 20-liter fermenter covered with 19 liters of sterile medium with the same final composition as the above-mentioned pre-cultivation; another 1.0 ml foam is added to reduce foaming;

[0078] After 12 hours of growth period at an overpressure of 0.4~0.6bar and a temperature of 26±1℃, aeration at 4L / min and stirring at 165rpm;

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

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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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