Method for preparing high-purity fenofibric acid in phase transfer catalysis method

A technology of phase transfer catalysis and fenofibric acid, which is applied in the field of catalytic synthesis of fenofibric acid, can solve the problems of large amount of acetone, acid and alkali, and high impurities, so as to reduce use and consumption, reduce solvent loss, and avoid The effect of rectification recovery

Inactive Publication Date: 2018-08-10
XUZHOU COLLEGE OF INDAL TECH
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0005] The invention provides a method for preparing high-purity fenofibric acid by a phase-transfer catalysis method, which is used to solve the problem of large amount of acetone used in the prior art and difficult recovery, long reaction time, repeated pH adjustment with acid, repeated fil

Method used

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  • Method for preparing high-purity fenofibric acid in phase transfer catalysis method

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Embodiment 1

[0029] Add 60 g of water I and 40 g of sodium hydroxide to a four-necked flask equipped with electric stirring, a thermometer, a reflux condenser, and a constant pressure dropping funnel at a speed of 400 r / min, cool down to 40°C, add 50 g of toluene I, 55 g of acetone, 4 -Hydroxy-4'-chlorobenzophenone 40g, PEG-400, 4g; add chloroform 28g dropwise at 47±1°C, keep warm at 47±1°C for 0.5 h after the dropwise addition, and then heat at 59-60°C Incubate for 2 h; add 40 g of water II to the reaction solution, filter, add 55 g of toluene II to the filtrate, acidify with hydrochloric acid (53 g) to pH = 2, then add 55 g of water III to promote the complete dissolution of salts, and let stand to separate the lower water layer , heating the upper layer material liquid to 66±1°C, adding 60g of water IV to cool down to 33°C, standing to separate the lower layer water layer, filtering the upper layer material liquid, washing the filter cake with water until the filtrate pH=6, and obtaining...

Embodiment 2

[0031] Add 55g of water I and 45g of sodium hydroxide into a four-neck flask equipped with electric stirring, thermometer, reflux condenser, and constant pressure dropping funnel at a speed of 450r / min, cool down to 40°C, add 55g of toluene I, 55g of acetone, 4 -Hydroxy-4'-chlorobenzophenone 40g, PEG-400, 3g; add chloroform 32g dropwise at 48±1°C, keep warm at 48±1°C for 0.5 h after the dropwise addition, and then heat at 58-59°C Incubate for 2.5 h; add 50 g of water II to the reaction solution, filter, add 50 g of toluene II to the filtrate, acidify with hydrochloric acid (51 g) to pH = 3, then add 60 g of water III to promote the complete dissolution of salts, and let stand to separate the lower water layer , heating the upper layer material liquid to 68±1°C, adding 50g of water IV to cool down to 35°C, standing to separate the lower layer water layer, filtering the upper layer material liquid, washing the filter cake with water until the filtrate pH=7, and obtaining the wet ...

Embodiment 3

[0033] Add 58g of water I and 42g of sodium hydroxide into a four-necked flask equipped with electric stirring, thermometer, reflux condenser, and constant pressure dropping funnel at a speed of 450r / min, lower the temperature to 40°C, add 60g of toluene I, 60g of acetone, 4 -Hydroxy-4'-chlorobenzophenone 40g, PEG-400, 5g; add chloroform 30g dropwise at 49±1°C, keep warm at 49±1°C for 0.5 h after the dropwise addition, and then heat at 58-59°C Incubate for 2.5 h; add 45 g of water II to the reaction solution, filter, add 60 g of toluene II to the filtrate, acidify with hydrochloric acid (54 g) to pH = 2, then add 50 g of water III to promote the complete dissolution of salts, and let stand to separate the lower water layer , heating the upper material liquid to 69±1°C, adding 55g of water IV to cool down to 32°C, standing to separate the lower water layer, filtering the upper layer material liquid, washing the filter cake with water until the filtrate pH=7, and obtaining the we...

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Abstract

The invention discloses a method for preparing high-purity fenofibric acid in a phase transfer catalysis method, which belongs to the field of a fenofibric acid catalytic synthesis process. The methodcomprises the following steps: adopting 4-hydroxyl-4'-chlorobenzophenone, acetone and chloroform as raw materials, adopting a 40 percent sodium hydroxide solution as a catalyst, adopting PEG-400 as aphase transfer catalyst, adopting methylbenzene as a solvent, performing the condensation reaction, filtering, acidifying, separating the solution, heating, washing, filtering, washing, recrystallizing by virtue of absolute ethyl alcohol, and drying, thus obtaining the high-purity fenofibric acid. By adopting the method, the use and consumption of precursor chemical acetone can be greatly reduced, the loss of the solvent is significantly reduced, less waste is produced, and the method is a green method for synthesizing fenofibric acid and is suitable for the industrialized production.

Description

technical field [0001] The invention relates to a preparation method of fenofibric acid, in particular to a method for preparing high-purity fenofibric acid by a phase transfer catalysis method, belonging to the technical field of fenofibric acid catalytic synthesis. Background technique [0002] Fenofibric acid is an important intermediate for the synthesis of the blood lipid-lowering drug fenofibrate. It has a wide range of uses and is usually obtained through condensation reactions using 4-hydroxy-4'-chlorobenzophenone, acetone and chloroform as raw materials. [0003] Regarding the synthesis of fenofibric acid at present, most of the bibliographical reports take 4'-chloro-4-hydroxybenzophenone as raw material, under alkaline conditions with chloroform or 2-bromoisobutyric acid and acetone or butanone A condensation reaction occurs to generate fenofibric acid. In the existing synthesis technology, the yield of fenofibric acid crude product is low, and it needs multiple c...

Claims

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Application Information

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IPC IPC(8): C07C51/00C07C51/02C07C59/90
CPCC07C51/00C07C51/02C07C59/90
Inventor 孙婷婷李敢王德堂祁娟徐彦红
Owner XUZHOU COLLEGE OF INDAL TECH
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