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A kind of preparation method of testosterone propionate
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A technology of testosterone propionate and hydroxyandrosterol, applied in the field of drug preparation, can solve the problems of excessive waste water, low yield, large impurities, etc., and achieve the effects of less environmental pollution, high purity, and high product quality and yield
Active Publication Date: 2021-12-21
ZHEJIANG SHENZHOU PHARMA
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[0006] In order to solve the problems of large impurities, low yield, and a lot of waste water in the preparation process of testosterone propionate in the prior art, the invention provides a green and environment-friendly preparation method of testosterone propionate
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example 1
[0021] Example 1 Preparation of testosterone propionate
[0022] Under a nitrogenatmosphere, 10g of testosterone (17p-hydroxy-androst-4-en-3-one) were charged to a 10ml of dichloromethane, 1ml of pyridine was added, 5g 4- dimethylaminopyridine (of DMAP), propionic anhydride was added 10ml , incubated 20 ℃ the reaction to completion, water was added, layered, washing, concentration, filtration, and dried to obtain 11.1 g of testosterone propionate, yield 111%, purity: 98.9%.
example 2
[0023] Example 2 Preparation of testosterone propionate
[0024] Under an argonatmosphere, 10g of testosterone (17p-hydroxy-androst-4-en-3-one) were charged to 100ml of dichloroethane, was added 100ml of triethylamine, 10g 4- dimethylaminopyridine (DMAP) was , 50ml propionic anhydride was added, incubated 50 deg.] C until complete reaction, water was added, layered, washing, concentration, filtration, and dried to obtain 11.2 g of testosterone propionate, yield 112%, purity: 98.8%.
example 3
[0025] Example 3 Preparation of testosterone propionate
[0026] Under heliumatmosphere, 10g of testosterone (17p-hydroxy-androst-4-en-3-one) were charged to a 200ml of dichloromethane was added diisopropylethyl amine 50ml, 0.01g 4- dimethylaminopyridine (of DMAP), propionic anhydride was added 4.5ml, incubated 80 deg.] C until complete reaction, water was added, layered, washing, concentration, filtration, and dried to obtain 11.1 g of testosterone propionate, yield 111%, purity: 98.7%.
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Abstract
The invention discloses a preparation method of testosteronepropionate, which belongs to the technical field of preparation and processing of medicines. In the method, testosterone is used as a raw material, and through the catalysis of a catalyst, an organic base is used as an acid-binding agent to undergo esterification reaction with propionic anhydride to obtain testosteronepropionate. The method of the present invention avoids the use of expensive and highly toxic acid chlorides, and the solvent used is water-insoluble, so after the reaction is completed, the product can be directly layered and extracted without adding water to separate out the product, reducing the consumption of water, and the solvent can be Recycling and reuse makes the whole process more environmentally friendly; the reaction product of the invention has high purity, easy purification, product quality and yield higher than 110%, is suitable for industrialized large-scale production, and has good economic benefits.
Description
Technical field [0001] The present invention relates to the technical field of the preparation of a medicament, particularly relates to a method for preparing testosterone propionate. Background technique [0002] Testosteronepropionate belongs androgen drugs, clinically suitable for testis syndrome, cryptorchidism, male hypogonadism; menorrhalgia gynecological diseases, uterine fibroids; senile osteoporosis and aplastic anemia. [0003] The traditional method of preparation is the use of testosterone testosterone propionate as starting material in a solventpyridine, was added propionic anhydride, the reaction is about 60 ℃ 6 hours, a large number of water of precipitation, filtration, testosterone propionate to give the crude product in ethyl acetate and purified testosterone propionate obtained fine. This method uses pyridine as solvent, water precipitated materials after completion of the reaction, higher production costs, and cause a lot of waste water, polluting the enviro...
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