Extraction and purification method of 7 Alpha, 15Alpha-dihydroxy androstene alcohol ketone

A technology of hydroxyandrostenolone and purification method, applied in microorganism-based methods, biochemical equipment and methods, organic chemistry, etc., can solve problems such as inability to extract products, improve extraction efficiency, reduce production costs, and improve overall production. Yield effect

Inactive Publication Date: 2008-05-21
SHANGHAI INST OF PHARMA IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This shows that the existing extraction method can not effectively extract the product

Method used

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  • Extraction and purification method of 7 Alpha, 15Alpha-dihydroxy androstene alcohol ketone
  • Extraction and purification method of 7 Alpha, 15Alpha-dihydroxy androstene alcohol ketone
  • Extraction and purification method of 7 Alpha, 15Alpha-dihydroxy androstene alcohol ketone

Examples

Experimental program
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Effect test

Embodiment 2

[0032] 1 L of fermentation broth with a substrate feeding concentration of 8 g / L and a conversion rate of 85.1% was centrifuged (rotating at 4000 rpm for 15 minutes). The supernatant was extracted with 1 L of propyl acetate; 0.24 kg of bacteria were first added to 1.2 L of 100% methanol at room temperature, stirred and soaked for 4 hours, then filtered, and the bacteria were extracted again with 0.8 L of 100% methanol in the same way. The methanol solutions obtained from the two extractions were mixed, and the organic solvent in the solution was distilled off, and then extracted with 3 L and 2 L of propyl acetate successively. All extracts were combined, and 10 g of anhydrous sodium sulfate was added to remove water. Then distill off most of the ethyl acetate to about 200ml, cool to room temperature and let stand for 2 hours, then filter the obtained solid to wash with 20ml of pre-cooled propyl acetate, then heat to dissolve with 30ml of methanol, and then add 200ml of 4-methy...

Embodiment 3

[0034]1 L of fermentation broth with a substrate feeding concentration of 8 g / L and a conversion rate of 85.1% was centrifuged (rotating at 4000 rpm for 15 minutes). The supernatant was extracted with 1 L of propyl acetate; 0.24 kg of bacteria were first added with 1.2 L of 100% ethanol at room temperature, stirred and soaked for 4 hours, then filtered, and the bacteria were extracted again with 0.8 L of 100% ethanol. The ethanol solutions obtained from the two extractions were mixed, and the organic solvent in the solution was distilled off, and then extracted with 3 L and 2 L of propyl acetate successively. All extracts were combined, and 10 g of anhydrous sodium sulfate was added to remove water. Then distill off most of the ethyl acetate to about 200ml, cool to room temperature and let stand for 2 hours, then filter the obtained solid to wash with 20ml of pre-cooled propyl acetate, then heat to dissolve with 30ml of methanol, and then add 200ml of 4-methyl-2- For pentanon...

Embodiment 4

[0036] 1 L of fermentation broth with a substrate feeding concentration of 8 g / L and a conversion rate of 85.1% was centrifuged (rotating at 4000 rpm for 15 minutes). The supernatant was extracted with 1 L of ethyl acetate; the cells were first extracted with 2 L of 85% acetone solution, and then extracted with 0.6 L of 85% acetone solution. Others were the same as in Example 1, and finally 5.89 g of a product with a purity of 98.5% was obtained.

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Abstract

The invention provides a method for extracting and purifying 7α, 15α-dihydroxyandrostenolone. The 7α, 15α-dihydroxyandrostenolone is prepared from dehydroepiandrosterone through the biological process of Colletotrichum lini AS 3.4486. obtained by transformation, after the transformation is completed, the fermentation liquid is centrifuged, and the supernatant is extracted with a non-polar organic solvent. The steps of organic solvent extraction. Using this method for extraction and purification, the yield of the product can reach nearly 90%, and the total yield of I prepared by conversion of dehydroepiandrosterone can reach 75%, thereby effectively improving the total yield of I by conversion of dehydroepiandrosterone. Yield, reducing the production cost of I.

Description

technical field [0001] The present invention relates to a method for extracting and purifying a biotransformation product from a fermentation broth, in particular to a method for effectively converting a substrate dehydroepiandrosterone into a product 7α, 15α-dihydroxyandrostenolone from a fermentation broth Methods of extracting and purifying the product. Background technique [0002] Steroid intermediates are often used in the production of various clinical drugs. 7α, 15α-dihydroxyandrostenolone and its analogs (its structure is as follows: Formula I) [0003] [0004] It is an important steroid intermediate, which can be used in the synthesis of various drugs such as lactone aldosterone receptor antagonists, diuretics and gynecological drugs. For example, I is an important intermediate in the synthesis of drospirenone, the active ingredient of the oral contraceptive drug Yasmin. [0005] Microbial transformation plays an important role in the synthesis of steroid dr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C12P33/06C07J1/00C12R1/645
Inventor 胡海峰陶荣盛张琴
Owner SHANGHAI INST OF PHARMA IND CO LTD
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