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Purification technology of pregnenolone acetate

A technology for pregnenolone acetate and pregnenolone alcohol, which is applied in directions such as organic chemistry and steroids, can solve problems such as high cost, influence on the production and application of pregnenolone alcohol, and achieves the effect of easy operation.

Active Publication Date: 2011-02-16
SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In any case, because pregnenone alcohol is not yet a bulk commodity, and the cost of small-scale purification of the crude product of pregnenone alcohol is too high, it directly affects the production and application of the technology of using hydrogen peroxide instead of chromic anhydride to produce pregnenone alcohol

Method used

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  • Purification technology of pregnenolone acetate
  • Purification technology of pregnenolone acetate
  • Purification technology of pregnenolone acetate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Synthesis and purification of embodiment 1 compound 2a

[0019]

[0020] Put 50 g of pregna-16-en-20-one-3-ol crude product (content 88%) in a dry 1 liter three-neck reaction flask, add 120 ml of acetic anhydride, and heat to dissolve. After reacting at 100°C for 1 h, the acetylation reaction was complete. After cooling the reaction temperature, 150 ml of water was added to decompose excess acetic anhydride. Then, extract with cyclohexane at 50° C. in portions, 300 ml each time, and extract 5 times in total. The extracts were combined, cyclohexane was recovered under reduced pressure, and 40 g of the product was obtained by recrystallization from ethanol, with a content of 97.1% and a yield of 78%.

Embodiment 2

[0021] Synthesis and purification of embodiment 2 compound 2a

[0022]

[0023] Put 50 g of the crude product of pregna-16-en-20-one-3-ol (content 85%) in a dry 1 liter three-neck reaction flask, add 100 ml of acetic anhydride, and heat to dissolve. After 45 min at reflux temperature, the acetylation reaction was complete. After cooling the reaction temperature, 100 ml of water was added to decompose excess acetic anhydride. Then, extract with 60°C hot cyclohexane in batches, 250ml each time, and extract 6 times in total. The extracts were combined, cyclohexane was recovered under reduced pressure, and then recrystallized with ethanol to obtain 37.4 g of the product with a content of 96.5% and a yield of 75%.

Embodiment 3

[0024] Synthesis and purification of embodiment 3 compound 2a

[0025]

[0026] Put 50 g of the crude product of pregna-16-en-20-one-3-ol (content 82%) in a dry 1 liter three-neck reaction flask, add 80 ml of acetic anhydride, and heat to dissolve. After reacting at 120°C for 1.5h, the acetylation reaction was complete. After cooling the reaction temperature, 100 ml of water was added to decompose excess acetic anhydride. Then, use 60°C hot petroleum ether to extract in portions, 260ml each time, and extract 7 times in total. The extracts were combined, petroleum ether was recovered under reduced pressure, and 35.7 g of the product was obtained by recrystallization with methanol, with a content of 96.2% and a weight yield of 74%.

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Abstract

The invention relates to an environment-friendly production method of pregnenolone acetate. By using the method, various impurities can be separated and removed from coarse pregnenolone products synthesized by an oxydol oxidative degradation method, and pure pregnenolone acetate products with high yield and high purity can be synthesized from the oxydol oxidative degradation method-synthesized coarse pregnenolone products. The technology solves the problem on product purification in the synthesis of pregnenolone acetate compounds using oxydol to replace chromic anhydride, and enables the pregnenolone synthesis method using oxydol to replace chromic anhydride to be more applicable to industrial production. The method for producing pregnenolone acetate has the advantage of convenient operation and is applicable to mass production.

Description

technical field [0001] The invention relates to a purification technology of pregnenol acetate. With the method of the present invention, various impurities in the crude pregnenone alcohol synthesized by the hydrogen peroxide oxidative degradation method can be easily separated and removed, and the crude pregnenone alcohol synthesized by the hydrogen peroxide oxidative degradation method can be obtained with high yield and high purity. The product is a pure product of pregnenol acetate. This technology solves the product purification problem when hydrogen peroxide is used instead of chromic anhydride to synthesize pregnenone alcohol compound, making the invented method of using hydrogen peroxide instead of chromic anhydride to synthesize pregnenone alcohol more suitable for industrial production applications. Because the method for producing pregnenol acetate is easy to operate, it is suitable for mass production. technical background [0002] Pregnenol acetate includes pr...

Claims

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Application Information

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IPC IPC(8): C07J13/00
Inventor 田伟生汪昀
Owner SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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