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A clean production preparation method of testosterone propionate

A technology of testosterone propionate and clean production, which is applied in the field of clean production and preparation of testosterone propionate, which can solve the problems of large amount of waste acid water, low purity of testosterone propionate, and high processing cost, so as to reduce recycling and realize clean production , the effect of reducing environmental pollution

Active Publication Date: 2022-03-25
湖北竹溪人福药业有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the problems in the prior art that the purity of testosterone propionate is not high, the amount of waste acid water is large, and the treatment cost is high, the present invention proposes a clean production method for testosterone propionate

Method used

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  • A clean production preparation method of testosterone propionate
  • A clean production preparation method of testosterone propionate
  • A clean production preparation method of testosterone propionate

Examples

Experimental program
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Effect test

Embodiment 1

[0024] (1) Add 60g of propionic acid and 10g of testosterone into the reaction bottle, stir well, add 3g of propionyl chloride, heat up to reflux for 3 hours, monitor by TLC, the reaction is complete; add 600g of water into the beaker, stir the reaction solution in the reaction bottle slowly Add dropwise into water, stir evenly, filter with suction, wash the material with 200g of water until the pH is 6, drain and discharge the material, dry to obtain 11.7g of testosterone propionate crude product, and collect a total of 850g of waste acid water at the same time;

[0025] (2) Add 117g of methanol, 0.351g of activated carbon, and 11.7g of crude testosterone propionate into the reaction flask, heat up and reflux for decolorization for 1 hour, filter with suction, concentrate the filtrate to the remaining 11.7g of methanol, cool down to 5°C, stir and crystallize for 4 hours, and vacuum filter , drained and discharged, dried at 60°C to constant weight to obtain 11.3g of testosteron...

Embodiment 2

[0028] (1) Add 80g of propionic acid and 10g of testosterone into the reaction bottle, stir well, add 5g of propionyl chloride, heat up to reflux for 2 hours, monitor by TLC, the reaction is complete; add 800g of water into the beaker, stir the reaction solution in the reaction bottle slowly Add dropwise into water, stir evenly, filter with suction, wash the material with 300g of water until the pH is 7, drain and discharge the material, and dry to obtain 11.5g of testosterone propionate crude product, while collecting a total of 1170g of waste acid water;

[0029] (2) Add 138g of methanol, 0.575g of activated carbon, and 11.5g of crude testosterone propionate into the reaction flask, heat up and reflux for decolorization for 0.5h, filter with suction, concentrate the filtrate to the remaining 17.25g of methanol, cool down to 0°C, stir and crystallize for 2h, filter , drained and discharged, dried at 65°C to constant weight to obtain 11.2g of testosterone propionate with a puri...

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Abstract

The invention discloses a clean production and preparation method of testosterone propionate. The method uses testosterone as a raw material, undergoes esterification and refining to obtain testosterone propionate with a product purity ≥ 99.5%, and the waste acid water produced in the preparation process is passed through sodium carbonate Neutralization, activated carbon decolorization, suction filtration and concentration, the by-product sodium propionate is prepared, which reduces the pollution of waste water to the environment. While preparing high-purity testosterone propionate, the present invention effectively recycles components in waste acid water to obtain by-product sodium propionate, thereby reducing costs and realizing clean production of testosterone propionate.

Description

technical field [0001] The invention belongs to the technical field of steroid medicine preparation, and in particular relates to a clean production preparation method of testosterone propionate. Background technique [0002] Testosterone propionate, also known as testosterone propionate, androgen drugs, clinically applicable to anorchidism, cryptorchidism, male hypogonadism; gynecological diseases such as menorrhagia, uterine fibroids; senile osteoporosis and regeneration Obstructive anemia, etc. [0003] According to retrieval, it is mentioned in the preparation method of testosterone propionate that testosterone is reacted with propionic anhydride to carry out acylation synthesis. In the process of realizing the present invention, the inventor finds that at least the following problems exist in the prior art: , testosterone's 3-ketone group and 17-hydroxyl group will simultaneously generate diester impurities, and after the reaction, the water will be analyzed, and propi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J1/00
CPCC07J1/0025
Inventor 侯海波杨艳青郑建雄张阳洋赵静刘林李廿罗宇肖康狄飞飞蔡啸
Owner 湖北竹溪人福药业有限责任公司
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