Purification method for progesterone

A purification method and progesterone technology, which is applied in the purification of progesterone crude product and the field of progesterone purification, can solve the problems that it is difficult to produce qualified progesterone raw material medicine and reduce it to below 0.6%, and achieve good economic and social benefits , low equipment requirements, simple and convenient operation

Active Publication Date: 2021-02-23
ZHEJIANG SHENZHOU PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The content of bisnoraldehyde in crude progesterone is 2-3%. It is impossible to reduce the impurity content below 0.6% through general refining methods, and it is difficult to produce qualified progesterone raw materials that meet the European Pharmacopoeia

Method used

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  • Purification method for progesterone
  • Purification method for progesterone

Examples

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Comparison scheme
Effect test

example 1

[0041] The high-purity purification method of example 1 progesterone

[0042] Put 50g of crude progesterone (containing 2% impurity aldehyde) into 50ml of ethanol, add 2.5ml of 40% sodium metabisulfite aqueous solution, control 60°C to stir and react for 1 hour after completely dissolving, cool to 5°C, and obtain a preliminary reaction treatment product.

[0043] Add 25ml of water to the preliminary reaction product, filter, wash the filter cake with water until neutral, and dry to obtain 47.8g of progesterone fine product, the product yield is 95.6%, the product melting point is 129.0-130.0°C, the HPLC content is 99.6%, and the impurity aldehyde figure 2 mentioned.

[0044] The high performance liquid chromatogram of this progesterone crude product is as follows figure 1 shown.

example 2

[0045] The high-purity purification method of example 2 progesterone

[0046] Put 50g of crude progesterone (containing 3% impurity aldehyde) into 350ml of isopropanol, add 25ml of 20% potassium bisulfite aqueous solution, completely dissolve, control 40°C to stir and react for 0.1 hour, cool down to -5°C, and obtain the preliminary reaction treatment product .

[0047] Add 150ml of water to the preliminary reaction product, filter, wash the filter cake until neutral, and dry to obtain 47.6g of progesterone fine product, the product yield is 95.2%, the product melting point is 129.1-130.0°C, the HPLC content is 99.5%, and the impurity aldehyde is <0.2% .

example 3

[0048] The high-purity purification method of example 3 progesterone

[0049] Put 50g of progesterone crude product (containing 3% impurity aldehyde) into 750ml of tert-butanol, add 50ml of 5% potassium metabisulfite aqueous solution, control 20°C to stir and react for 2 hours after completely dissolving, cool down to -20°C, and obtain the preliminary reaction treatment product .

[0050] Add 250ml of water to the preliminary reaction product, filter, wash the filter cake until neutral, and dry to obtain 47.5g of progesterone fine product, the product yield is 95.0%, the product melting point is 129.1-130.2°C, the HPLC content is 99.6%, and the impurity aldehyde <0.15% .

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Abstract

The invention discloses a purification method for progesterone, belonging to the technical field of preparation and processing of steroid hormone drugs. According to the method, aldehyde impurities ina progesterone crude product react with a sulfur-containing nucleophilic reagent to generate high-polarity hydroxyl sulfonate, the high-polarity hydroxyl sulfonate and progesterone are subjected to solubility differentiation, and then high-purity progesterone with the content higher than 99.5% and the total content of impurity aldehyde lower than 0.2% is obtained through water adding, water precipitation, filtering, filter cake washing and drying. According to the purification method, technical bottlenecks in progesterone purification in the prior art are avoided, all the reagents and raw materials used in the reaction process are low in price and easy to obtain; purification process is easy and convenient to operate, requirements on equipment is low, and cost investment is small; a purification process is mild and safe, conditions are easy to control, and the purification and recovery rate of products is high; the used reagents are low in environmental pollution, and in particular, chromium-containing high-pollution reagents are not used, so the industrial development trend of green chemistry is met; and the method has good economic and social benefits.

Description

technical field [0001] The invention relates to the technical field of preparation and processing of steroid hormone drugs, in particular to a method for purifying progesterone, in particular to a method for purifying crude progesterone containing aldehyde impurities. Background technique [0002] Progesterone is a natural progesterone secreted by the corpus luteum of the ovary. It has a significant morphological effect on the endometrium stimulated by estrogen in the body. It is necessary to maintain pregnancy and has a very important use in clinical medicine. [0003] There are many methods for synthesizing progesterone with bisbutanol as the starting material. [0004] Method A first oxidizes bisnoraldehyde to bisnoraldehyde, and then obtains progesterone through catalytic oxidation, and its synthetic route is as follows: [0005] [0006] In the catalytic oxidation process of this method, it is difficult to completely convert bisnoraldehyde, so the final product prog...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J7/00
CPCC07J7/002C07J9/00C07J31/006
Inventor 邵振平王荣王炳乾王洪福黄橙橙雷灵芝王友富
Owner ZHEJIANG SHENZHOU PHARMA
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