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A kind of purification method of progesterone

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

Active Publication Date: 2021-09-28
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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  • A kind of purification method of progesterone
  • A kind of purification method of progesterone
  • A kind of purification method of progesterone

Examples

Experimental program
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 method for purifying progesterone, which belongs to the technical field of preparation and processing of steroid hormone drugs. The method utilizes the aldehyde impurities in the crude progesterone to react with sulfur-containing nucleophiles to generate highly polar hydroxysulfonate and progesterone to achieve solubility differentiation, and then add water for water analysis, filter, wash the filter cake with water, and dry to obtain High-purity progesterone with a content higher than 99.5% and a total impurity aldehyde content lower than 0.2%. The purification method of the present invention avoids the technical bottleneck of progesterone purification in the prior art, and the raw materials of the reagents used in the reaction process are cheap and easy to obtain, the purification process is simple and convenient to operate, low in equipment requirements, and low in cost investment; the purification process Mild, safe, easy to control conditions, high recovery rate of product purification; the reagents used have little environmental pollution, especially do not use chromium-containing highly polluting reagents, which is in line with the industrial development trend of green chemistry and 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 Patents(China)
IPC IPC(8): C07J7/00
CPCC07J7/002C07J9/00C07J31/006Y02P20/55
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