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Preparation method of dehydroepiandrosterone

A technology of dehydroepiandrosterone and dehydroepiandrosterone acetate, which is applied in the field of improvement of synthesis process, can solve problems such as low yield, achieve the effects of reducing damage, reducing the use of toxic reagents, and reducing costs

Inactive Publication Date: 2012-07-25
YICHENG GOTO PHARMA
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Problems solved by technology

[0004] The purpose of the present invention is exactly to solve the shortcoming that the yield of existing production method is low, provides the synthetic method that reaction condition is easy to control, simple to operate, pollution is little, dienolone acetate is synthesized dehydroepiandrosterone, and yield reaches 70.0 % dehydroepiandrosterone synthesis method

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  • Preparation method of dehydroepiandrosterone

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Embodiment Construction

[0026] The present invention will be further described below in conjunction with specific examples 1-5, but the present invention is not limited.

[0027] Table 1 shows the purity and yield of raw materials used in the present invention, acetic acid gestational dienol ketone oxime obtained through oximation reaction, and dehydroepiandrosterone acetate obtained through Beckmann rearrangement hydrolysis reaction.

[0028] The present invention prepares the processing step of testosterone enanthate as follows:

[0029] (1) Oximation reaction: Pregnant acetic acid dienolone: ​​sodium acetate: absolute ethanol = 1: 1.35: 4.2; add acetic acid pregnant dienolone, sodium acetate, and absolute ethanol to the reaction tank, heat and reflux for 4 hours, and cool down To 40±5°C, add 4 times the amount of water, the product is precipitated, centrifuged, and dried to obtain acetic acid pregnant dienolketoxime;

[0030] ⑵, Beckman rearrangement hydrolysis reaction: the feed ratio is acetic ...

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Abstract

The invention discloses a preparation method of dehydroepiandrosterone, belongs to the technical field of medicine intermediate preparation, and is mainly used for solving the problems of higher production cost, low product yield and more serious pollution existing in the traditional dehydroepiandrosterone synthesis method. The preparation method comprises the following process steps of: (1) oximation reaction: subjecting 16-dehydropregnenolone acetate, sodium acetate and absolute ethyl alcohol with the ratio of 1:(1.2-1.5):(4-4.5) to oximation reaction to obtain 16-dehydropregnenolone acetate oxime; (2) Beckmann rearrangement hydrolysis reaction: charging the 16-dehydropregnenolone acetate oxime, chloroform, phosphorus pentoxide, hydrochloric acid and water with the ratio of 1:(6-6.5):(0.8-1.0):(0.5-0.8):(6-7.0) to obtain dehydroepiandrosterone acetate; and (3) hydrolysis reaction: charging a crude dehydroepiandrosterone acetate, methanol, potassium carbonate, hydrochloric acid, methanol and active carbon with the ratio of 1:(7.0-8.0):(0.4-0.5):(0.3-0.4):(5.0-6.0):(0.4-0.5) to obtain dehydroepiandrosterone. The preparation method has the characteristics of easiness in reaction condition control, simplicity in operation, little pollution and high yield and is mainly used for preparing dehydroepiandrosterone.

Description

technical field [0001] The invention belongs to the technical field of preparation of pharmaceutical intermediates. In particular, it relates to the improvement of a specific synthesis process of dehydroepiandrosterone. Background technique [0002] Dehydroepiandrosterone (DHEA) is an important physiologically active substance secreted by the human body, which plays an extremely important role in maintaining normal physical and sexual functions and prolonging human physiological and psychological life. The secretion of DHEA in the human body reaches its peak at the age of 25 to 30, and then declines year by year. The content in the body around the age of 70 can only reach 5% to 10% of the peak period. A large number of clinical experiments have confirmed that a high level of DHEA in the human body leads to good physical fitness and strong disease resistance; otherwise, physical decline, weak disease resistance, and accelerated aging of the human body. It is mainly used as ...

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Application Information

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IPC IPC(8): C07J1/00
Inventor 系祖斌张国俊王延贞
Owner YICHENG GOTO PHARMA
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