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Method for purifying temsirolimus

A technology of temsirolimus and purification method, applied in the direction of organic chemistry, etc., can solve the problems of being unsuitable for industrial production, unable to meet industrialization requirements, and high cost of high-efficiency liquid phase systems, and achieves small complexes, mild conditions, and processes. simple effect

Inactive Publication Date: 2018-12-07
LUNAN PHARMA GROUP CORPORATION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

CN104086564A discloses a method for purifying temsirolimus, which uses high-performance liquid chromatography to remove impurities in the crude product. Although the purity of this method can meet the quality requirements, the cost of using a high-performance liquid phase system is relatively high, which is not suitable for Industrialized production cannot meet the requirements of industrialization

Method used

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  • Method for purifying temsirolimus

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Effect test

Embodiment 1

[0022] Weigh 200g of 200-300mesh silica gel, soak it in petroleum ether and put it into a chromatography column for use; weigh 30g of temsirolimus crude product (purity 85.4%, maximum simple impurity 6.2%), dissolve it in 120ml ethyl acetate, load , after loading the sample, use 1800ml volume ratio of 1:1, 1:2, 2:5 mixed solution of petroleum ether and ethyl acetate to elute the impurities, then use ethyl acetate to elute and collect Division of the solution; maintain 20 ~ 25 ° C, the vacuum degree is not lower than -0.09Mpa conditions under reduced pressure to concentrate the collected solution to obtain 24.6 g of light yellow foamy solid. In a 500ml three-necked flask, add 24.6g of light yellow solid and 148ml of ethyl acetate obtained above, heat up to 30°C, stir to dissolve, add 2.5g of activated carbon, continue stirring for 30min and filter; transfer the filtrate into a 1000ml three-necked flask, stir slowly and drop Add 248ml of petroleum ether, slowly cool down to -10~...

Embodiment 2

[0024] Weigh 200g of 200-300 mesh silica gel, soak it with petroleum ether and put it into a chromatography column for use; weigh 30g of temsirolimus crude product (purity 85.4%, maximum simple impurity 6.2%) and dissolve it in 120ml dichloromethane, load the sample , after loading the sample, use 1800ml volume ratio of 1:1, 1:2, 2:5 mixed solution of petroleum ether and ethyl acetate to elute the impurities, then use ethyl acetate to elute and collect Division of the solution; maintain 20 ~ 25 ° C, the vacuum degree is not lower than -0.09Mpa conditions under reduced pressure to concentrate the collected solution to obtain 25.4 g light yellow foamy solid. In a 500ml three-necked flask, add 25.4g of the light yellow solid obtained above and 203ml of acetone, heat up to 25°C, stir to dissolve, add 2.6g of activated carbon, continue to stir for 30min and filter; transfer the filtrate to a 1000ml three-necked flask, stir and slowly add 305ml n-hexane, slowly lower the temperature...

Embodiment 3

[0026] Weigh 200g of 200-300 mesh silica gel, soak it with petroleum ether and put it into a chromatography column for use; weigh 30g of temsirolimus crude product (purity 85.4%, maximum simple impurity 6.2%) and dissolve it in 120ml dichloromethane, load the sample , after loading the sample, use 1800ml volume ratio of 1:1, 1:2, 2:5 mixed solution of petroleum ether and ethyl acetate to elute the impurities, then use ethyl acetate to elute and collect Division of the solution; maintain 20 ~ 25 ° C, the vacuum degree is not lower than -0.09Mpa conditions under reduced pressure to concentrate the collected solution to obtain 25.1 g light yellow foamy solid. In a 500ml three-necked flask, add 25.1g of the light yellow solid obtained above and 151ml of ethanol, heat up to 30°C, stir to dissolve, add 2.5g of activated carbon, continue to stir for 30min and filter; transfer the filtrate to a 1000ml three-necked flask, stir and slowly add 376ml Heptane, slowly cool down to -10~-5°C,...

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Abstract

The invention belongs to the field of pharmaceutical and chemical industry, and specifically discloses a method for purifying temsirolimus. The method comprises the following steps: preliminarily purifying a crude temsirolimus product through a silica gel column; then dissolving above-mentioned obtained temsirolimus in a solvent a, carrying out decolorization with active carbon, and carrying out filtering; dropwise adding a solvent b, carrying out cooling, and carrying out crystallization under stirring; and carrying out filtering, washing and vacuum drying so as to obtain a finished temsirolimus product. The temsirolimus purified by using the method provided by the invention has a purity of larger than or equal to 98.5% and a maximum single impurity of less than 0.2%; and the method for purifying the temsirolimus provided by the invention has simple process and is applicable to industrial production.

Description

technical field [0001] The invention belongs to the field of medicine and chemical industry, and in particular relates to a method for purifying temsirolimus. Background technique [0002] Renal cell carcinoma (RCC) is the most common type of renal cancer, and its incidence is second only to bladder cancer in urinary system tumors, accounting for 80-85% of adult renal malignant tumors. About 2-3% of all cancer patients are RCC patients, and 2% of all cancer-related deaths are caused by RCC. The International Cancer Society reported that the incidence of RCC is on the rise, with an increase of 2% every 10 years. [0003] [0004] The chemical name of Temsirolimus is rapamycin 42-[3-hydroxy-2-(hydroxymethyl)-2-methylpropionate], and the molecular formula is C 56 h 87 o 16 , the structural formula is shown in Formula 1. It is a targeted antineoplastic drug developed by Wyeth Medicine (now merged into Pfizer Medicine) for the treatment of advanced kidney cancer. It is al...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D498/18
CPCC07D498/18
Inventor 白文钦黄传青宋传玲
Owner LUNAN PHARMA GROUP CORPORATION
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