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Refining method for high-purity clofibric acid blood-lipid regulating drug--fenofibric acid

A technology of clofibric acid and fenofibric acid, which is applied in the field of medicine, can solve the problems of low product purity and consistent crystal form, and achieve the effect of easy transformation and production and low requirements for reaction equipment

Inactive Publication Date: 2014-08-06
肖广常
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the purity of the product obtained by this route is low, and the crystal form is difficult to keep consistent with the crystal form used in the marketed preparations

Method used

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  • Refining method for high-purity clofibric acid blood-lipid regulating drug--fenofibric acid
  • Refining method for high-purity clofibric acid blood-lipid regulating drug--fenofibric acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] (1) Organic solvent recrystallization: Add 400g of absolute ethanol and 50g of fenofibric acid into a 1000ml three-neck flask, reflux to dissolve, add 5g of activated carbon, decolorize for 30min, filter while hot, cool down to crystallize, filter, and dry at 60°C. 38 g of off-white solid was obtained, with a yield of 76% and a purity of 99.30%.

[0018] (2) Mixed solvent recrystallization: Add 140g of a mixed solvent of absolute ethanol and ethyl acetate (volume ratio 1:1) into a 250ml three-neck flask, then add 35g of the solid obtained in the previous step, reflux to completely dissolve, cool down and crystallize, Filter and dry at 60°C to obtain 24.6 g of off-white solid with a yield of 70.3% and a purity of 99.81%.

[0019] (3) Methanol recrystallization: add 160g of methanol and 20g of mixed solvent into a 250ml three-necked flask to recrystallize the off-white solid, reflux to completely dissolve, cool down to crystallize, filter, and dry at 60°C to obtain 15g of...

Embodiment 2

[0021] (1) Organic solvent recrystallization: Add 350g of acetone and 50g of fenofibric acid into a 1000ml three-necked flask, reflux to dissolve, add 5g of activated carbon, decolorize for 30min, filter while hot, cool down and crystallize, filter, and dry at 60°C to obtain White solid 35g, yield 70%, purity 99.36%.

[0022] (2) Mixed solvent recrystallization: Add 90g of a mixed solvent of absolute ethanol and ethyl acetate (volume ratio 1:1) into a 250ml three-neck flask, then add 30g of the solid obtained in the previous step, reflux to completely dissolve, and cool down to crystallize. Filter and dry at 60°C to obtain 22.2 g of off-white solid with a yield of 74% and a purity of 99.76%.

[0023] (3) Recrystallization of methanol: add 160g of methanol and 20g of mixed solvent into a 250ml three-neck flask to recrystallize the off-white solid, reflux to completely dissolve, crystallize at lower temperature, filter, and dry at 60°C to obtain 15.4g of white solid, yield 77%,...

Embodiment 3

[0025] (1) Organic solvent recrystallization: add 340g chloroform and 50g fenofibric acid into a 1000ml three-neck flask, reflux to dissolve, add 5g activated carbon, decolorize for 30min, filter while hot, cool down to crystallize, filter, dry at 60°C, 32 g of off-white solid was obtained, with a yield of 64% and a purity of 99.27%.

[0026] (2) Mixed solvent recrystallization: Add 100g of mixed solvent of n-propanol and ethyl acetate (volume ratio 1:1) into a 250ml three-neck flask, then add 30g of the solid obtained in the previous step, reflux to completely dissolve, cool down and crystallize, Filter and dry at 60°C to obtain 21 g of off-white solid with a yield of 70% and a purity of 99.78%.

[0027] (3) Recrystallization of methanol: add 160g of methanol and 20g of mixed solvent into a 250ml three-neck flask to recrystallize the off-white solid, reflux to completely dissolve, crystallize at lower temperature, filter, and dry at 60°C to obtain 15.2g of white solid, yield ...

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Abstract

The invention provides a refining method for a high-purity clofibric acid blood-lipid regulating drug--fenofibric acid and specifically relates to a method of three-step recrystallization of a crude fenofibric acid product for preparation of high-purity fenofibric acid, belonging to refining methods in the field of physics. According to the invention, the crude fenofibric acid product is subjected to organic solvent recrystallization, mixed solvent recrystallization and methanol recrystallization so as to prepare a finished fenofibric acid product. Solvents used in the method are frequently used solvents and are cheap and easily available, requirements on reaction equipment are low, so transformation production is facilitated. With the method, the finished fenofibric acid product with purity of no less than 99.9% can be obtained.

Description

Technical field: [0001] The invention belongs to the technical field of medicine. The present invention relates to a refined method for a high-purity clofibric acid derivative class blood lipid-regulating drug fenofibric acid, more specifically, relates to the process of obtaining high-purity fenofibric acid through three-step recrystallization of crude fenofibric acid new method. Background technique: [0002] Fenofibric acid is a blood lipid regulating drug derived from clofibric acid and is a metabolite of fenofibrate in vivo. Chinese name: fenofibric acid or fenofibric acid, English name: 2-(4-(4-chlorobenzoyl)phenoxy)-2-methyl-propanoic acid; chemical name: 2-[4-(4-chlorobenzoyl Acyl)phenoxy]-2-methylpropionic acid, the structural formula is as follows. [0003] [0004] Fenofibrate is a very poorly water-soluble active ingredient, its absorption in the digestive tract is limited, and its bioavailability is relatively low. Tenofibric acid is also the active form ...

Claims

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Application Information

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IPC IPC(8): C07C59/90C07C51/43
CPCC07C51/43
Inventor 王继鹏肖广常王建华
Owner 肖广常
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