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Preparation method for high-purity fenofibric acid crude drugs

A fenofibric acid, high-purity technology, applied in the synthesis method and refining field of fenofibric acid, can solve the problems of low yield, low product purity, and many times of refining, and achieve the effect of mild reaction conditions and simple operation

Inactive Publication Date: 2015-12-09
KANGYA OF NINGXIA PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These methods all have the disadvantages of low purity of crude product, low yield, many times of refining, and low product purity.

Method used

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  • Preparation method for high-purity fenofibric acid crude drugs
  • Preparation method for high-purity fenofibric acid crude drugs
  • Preparation method for high-purity fenofibric acid crude drugs

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Preparation of 4'-chloro-4-methoxybenzophenone (II)

[0032] Add 13.8g of anisole, 70ml of dichloromethane, and 25.5g of anhydrous aluminum trichloride into the reaction flask, stir at -5~0°C, add 29.0g of p-chlorobenzoyl chloride dropwise (with an equal volume of dichloro Diluted with methane), after dropping, the temperature was raised to room temperature for 2 hours, and the reaction was stopped. The reaction solution was added into ice water, stirred evenly, extracted with 50ml of dichloromethane to obtain a dichloromethane layer, evaporated to dryness to obtain a white solid, dried to constant weight, and weighed to obtain 29.3g, yield 93.2%.

[0033] Preparation of 4'-chloro-4-hydroxybenzophenone (I)

[0034] Add 29.0g of (II), 32.9g of anhydrous aluminum trichloride, and 90ml of chlorobenzene to the reaction flask in sequence. Cool at room temperature, concentrate to dryness at 70~90℃, -0.05~-0.085Mpa, let cool, add dichloromethane to dissolve, add ice water to...

Embodiment 2

[0055] Preparation of 4'-chloro-4-methoxybenzophenone (II)

[0056] Add 10.6g of anisole, 19.6g of anhydrous aluminum trichloride, and 60ml of dichloromethane into the reaction flask, stir at -10 to 0°C, add 22.3g of p-chlorobenzoyl chloride dropwise (with an equal volume of dichloromethane Diluted with methane), after dropping, the temperature was raised to room temperature and reacted for 3 hours, and the reaction was stopped. The reaction solution was added into ice water, stirred evenly, extracted with 50 ml of dichloromethane to obtain an organic layer, evaporated to dryness to obtain a white solid, dried to constant weight, and weighed to obtain 22.9 g, yield 94.6%.

[0057] Preparation of 4'-chloro-4-hydroxybenzophenone (I)

[0058] Add 12.6g of (II), 16.2g of anhydrous aluminum trichloride, and 40ml of chlorobenzene to the reaction bottle in sequence. After the addition, the temperature rises to 100°C. After heating and stirring for 2 hours, after the reaction is comp...

Embodiment 3

[0070] Preparation of 4'-chloro-4-methoxybenzophenone (II)

[0071] Add 13.2 g of anisole, 35 ml of anhydrous boron trifluoride ether solution, and 80 ml of dichloromethane into the reaction flask, stir at -10 to 0°C, add 25.6 g of p-chlorobenzoyl chloride dropwise (with an equal volume of dichloromethane Chloromethane dilution), dropwise, warming up to room temperature to react for 4 hours, stop the reaction. The reaction solution was added into ice water, stirred evenly, extracted with 60 ml of ethylene glycol monomethyl ether to obtain an organic layer, evaporated to dryness to obtain a white solid, dried to constant weight, and weighed to obtain 26.0 g, yield 85.6%.

[0072] Preparation of 4'-chloro-4-hydroxybenzophenone (I)

[0073] Add 15.3g of (II), 120ml of boron tribromide in methylene chloride (containing 50g of boron tribromide), and 50ml of chlorobenzene to the reaction flask in sequence. After the detection reaction is complete, place the reaction solution at ro...

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Abstract

The invention discloses a preparation method for fenofibric acid. According to the preparation method, with a compound expressed by the structural formula (I) being a raw material, the compound, acetone and chloroform are subjected to condensation reaction under the condition that sodium hydroxide serves as a catalyst to obtain fenofibric acid, and the structural formula (I) is shown as in the specification. In the structural formula (I), the expressed compound is 4'-chlorine-4-hydroxybenzophenone. The compound in the structural formula (I), acetone and chloroform are subjected to condensation reaction under catalyzing of sodium hydroxide, hydrolysis is performed through a sodium hydroxide solution, the pH value is adjusted two times, and then a fenofibric acid crude product is obtained; the crude product is recrystallized through isopropanol to obtain the high-purity fenofibric acid. The fenofibric acid product obtained through synthesis by the adoption of the method is high in yield and low in cost, and the preparation method is easy to implement and suitable for industrialized production.

Description

technical field [0001] The invention relates to a method for preparing medicine, in particular to a method for synthesizing and refining fenofibric acid. Background technique [0002] Fenofibric acid, Chinese chemical name: 2-[4-(4-chlorobenzoyl)phenoxy]-2-methylpropionic acid, English name: Fenofibricacid, CAS number: 42017-89-0, molecular formula: C 17 h 15 ClO 4 , molecular weight: 318.75, the structural formula is as follows: [0003] [0004] Clinical studies have shown that fenofibrate can lower cholesterol and blood lipids, and fenofibric acid is a metabolite of fenofibrate in vivo, which is a blood lipid regulating drug of clofibrate derivatives. The hydrophobicity of fenofibrate leads to its low bioavailability and is highly affected by food. In contrast to fenofibrate, fenofibric acid has a higher solubility in the small intestine area, thus increasing the bioavailability of fenofibric acid. availability, and bioavailability is not affected by food. [000...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C59/90C07C51/093C07C51/367C07C51/373C07C51/00
CPCC07C51/093C07C45/46C07C45/64C07C51/00C07C51/367C07C51/373
Inventor 李兆林杨亚军
Owner KANGYA OF NINGXIA PHARMA
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