Preparation method of testosterone enanthate

A technology of testosterone enanthate and testosterone, which is applied in the improvement field of synthesis process, can solve the problems of increased sewage treatment cost, high production cost, incomplete reaction and the like, and achieves the effects of less pollution, easy control of reaction conditions and simple operation.

Inactive Publication Date: 2012-07-11
YICHENG GOTO PHARMA
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Problems solved by technology

[0006] Although the method is simple, when the testosterone is obtained after reduction, the by-product diol is also obtained, and then the diol is oxidized, but the reaction is always incomplete, and 2.0% of the diol is not completely reacted.
In the process of synthesizing testosterone enanthate, the pr

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  • Preparation method of testosterone enanthate
  • Preparation method of testosterone enanthate
  • Preparation method of testosterone enanthate

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[0039] The present invention will be further described below in conjunction with specific examples 1-6, but the present invention is not limited.

[0040] The raw materials used in the present invention, the etherified product obtained through the etherification reaction, the testosterone through the reductive hydrolysis reaction, the purity and the yield are shown in Table 1.

[0041] The process steps of the present invention for preparing testosterone enanthate are as follows:

[0042] ⑴. Etherification reaction: pump absolute ethanol and triethyl orthoformate into the reaction tank, add 4-AD, and after dissolving, add pyridine hydrobromide, control the temperature to 42~45℃, and react for 8 hours; After the end, freeze the crystallization at 0±2℃ and centrifuge to obtain the etherate, or add triethylamine after the reaction, reduce the temperature and control the temperature at 0~5℃, keep the temperature and stir for 1 hour, at 0±2℃, freeze the crystallization , Centrifugation t...

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Abstract

The invention relates to a preparation method of testosterone enanthate, belonging to the technical field of preparation of testosterone enanthate and mainly solving the problems of the existing method of synthesis of testosterone enanthate that the side product diol is produced, the heptanoic anhydride is expensive, and the yield is low. The preparation method mainly comprises the following process steps of: (1) etherification: 4-AD, absolute ethyl alcohol, triethyl orthoformate and pyridine bromide hydrobromide are added according to the ratio of 1: (0.9-1.1): (0.7-0.9): (0.0045-0.0055), and ether compounds are prepared via etherification; (2) reduction and hydrolysis: etherate, sodium borohydride or potassium borohydride, methanol, hydrochloric acid and sodium hydroxide are added according to a ratio of 1: (0.12-0.18): (9-11): (0.8-1.2): (0.4-0.6), and testosterone is prepared via reduction and hydrolysis; and (3) halogenation: testosterone, benzene, pyridine, heptanoyl chloride, methanol and hydrochloric acid are added according to a ratio of 1: (5.8-6.2): (0.8-1.2): (0.75-0.85): (3.3-3.7): (0.5-0.7),and the testosterone enanthate is prepared via halogenation. The invention has the advantages that the reaction conditions can be controlled easily, the operation is simple, the product purity is high, the pollution is reduced, and the yield is high. The method is mainly applied in preparation of the testosterone enanthate.

Description

technical field [0001] The invention belongs to the technical field of testosterone enanthate preparation. In particular, it relates to the improvement of a specific synthesis process of testosterone enanthate. Background technique [0002] Testosterone enanthate is an important physiologically active substance secreted by the human body, which plays an extremely important role in maintaining normal physical and sexual functions, prolonging people's physical and psychological lifespan. It is mainly used for the replacement therapy of male hypogonadism, anorchidism, cryptorchidism or hypopituitarism and the treatment of advanced breast cancer. The pharmacological effects are: promote protein synthesis, inhibit protein decomposition, promote muscle growth, increase body weight, stimulate bone marrow red blood cell proliferation, etc. [0003] At present, the synthesis method of testosterone enanthate is generally as follows: 4-androstenedione (4-AD) is reduced to obtain test...

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Application Information

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IPC IPC(8): C07J1/00
Inventor 薛文武系祖斌王延贞
Owner YICHENG GOTO PHARMA
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