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Preparation method of bromfenac sodium dimer impurity

A technology of bromfenac sodium and dimer, applied in the field of medicine, can solve the problems such as no literature report on the preparation method of bromfenac sodium dimer impurity, and achieve the effects of efficient purification and purification, improved purity and high purity

Active Publication Date: 2015-01-07
GUANGDONG ZHONGSHENG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Bromfenac sodium dimer impurities are not sold in the domestic and foreign markets, and there is no bibliographical information on the preparation method of perbromfenac sodium dimer impurities, and bromfenac sodium bulk drugs and preparations need to pass the quality analysis when carrying out quality analysis. bromfenac sodium dimer impurities as a reference substance

Method used

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  • Preparation method of bromfenac sodium dimer impurity
  • Preparation method of bromfenac sodium dimer impurity
  • Preparation method of bromfenac sodium dimer impurity

Examples

Experimental program
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Effect test

Embodiment 1

[0038] The preparation of embodiment 1 bromfenac

[0039] In a 50L reactor, add 1.80kg of 7-(4-bromobenzoyl)-1,3-dihydro-indol-2-one, add 20L of 20% by mass aqueous sodium hydroxide solution, and heat to reflux React for 2-h, cool down, add dichloromethane for extraction, adjust the pH of the aqueous layer to 7.0 with acetic acid, filter, and dry at 50°C to obtain 1.46 kg of bromfenac, the purity of bromfenac is 82.99%, and bromfenac sodium dimer The content of impurities was 13.3%.

Embodiment 2

[0040] The preparation of embodiment 2 bromfenac sodium dimer impurity crude product

[0041] Take 100 g of bromfenac prepared in Example 1, add it to 400 mL of 50% by mass aqueous sodium hydroxide solution, heat up to 75° C. for 2 h, then continue to heat up to reflux for 3 h, then cool down to room temperature, and add acetic acid to adjust the pH to 6.5, crystallize, filter, wash the filter cake with 100mL of water, add to 200mL of ethyl acetate to make slurry for 1h, filter, collect the filtrate, concentrate under reduced pressure at 50°C, add acetonitrile to stir and crystallize, filter, and dry at 50°C to obtain 40.2g Bromfenac sodium dimer impurity crude product, the purity of bromfenac sodium dimer impurity is 77.05%, the HPLC figure of related substance is as follows figure 1 shown.

Embodiment 3

[0042] The preparation of embodiment 3 bromfenac sodium dimer impurity crude product

[0043] Take 100 g of bromfenac prepared in Example 1, add it to 350 mL of 45% by mass aqueous sodium hydroxide solution, heat up to 70°C for 3 hours, then continue to heat up to reflux for 4 hours, cool down to room temperature, and add acetic acid to adjust the pH to 5.5 , crystallization, filtration, the filter cake was washed with 100mL of water, added to 150mL of ethyl acetate for beating for 1h, filtered, the filtrate was collected, concentrated under reduced pressure at 50°C, added acetonitrile and stirred for crystallization, filtered, and dried at 50°C to obtain 39.6g of bromine Bromfenac sodium dimer impurity crude product, the purity of bromfenac sodium dimer impurity is 75.81%.

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Abstract

The invention belongs to the technical field of medicine, and provides a preparation method of a bromfenac sodium dimer impurity, which comprises the following steps: hydrolyzing 7-(4-bromobenzoyl)-1,3-dihydro-indolyl-2-one to obtain bromfenac, adding bromfenac into an alkali metal hydroxide solution, crystallizing to obtain a bromfenac sodium dimer impurity crude product, and adding the bromfenac sodium dimer impurity crude product into ethyl acetate to obtain the bromfenac sodium dimer impurity. The method can precipitate the impurity in the bromfenac sodium dimer impurity crude product by salification, simply and efficiently implements refinement and purification of the bromfenac sodium dimer impurity, enhances the purity to 99% above, is simple and convenient, and has the advantages of favorable environmental benefit and high yield.

Description

technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a preparation method of bromfenac sodium dimer impurities. Background technique [0002] Bromfenac sodium is one of the derivatives of 2-amino-3-benzoylphenylacetic acid, its chemical name is 2-amino-3-(4-bromobenzoyl)sodium phenylacetic acid, its structure is similar to that of ketoprofen and diclofenac Similarly, it can inhibit the synthesis of prostaglandin inflammatory mediators mediated by cyclooxygenase, and is the most effective cyclooxygenase inhibitor. It has a strong anti-inflammatory and analgesic effect, and its strength is 10 times that of other non-steroidal anti-inflammatory drugs. times. [0003] The disclosed bromfenac sodium preparation method mainly comprises following two kinds: 1. take 2-amino-4-bromobenzophenone and 2-methylthio ethyl acetate as raw materials, use aluminum chloride as catalyst, carry out Friedel -crafts acylation, followed by ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D487/04
CPCC07D487/04
Inventor 邓军谭珍友金联明黄爱君邵广志叶琼仙杜静
Owner GUANGDONG ZHONGSHENG PHARMA
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