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Imrecoxib purifying method

A purification method and pure product technology, applied in the field of purification of Erecoxib, can solve problems such as blocking and high difficulty of purification work

Pending Publication Date: 2019-04-02
JIANGSU HENGRUI MEDICINE CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, the existence of colored impurities has prevented those skilled in the art from obtaining high-quality Erecoxib bulk drug
In addition, during the preparation process, unknown simple impurities will occasionally appear in the product, and its HPLC retention time is about 7.901min (relative retention time is 1.13), and the retention time of Erecoxib HPLC is about 7.009min. Brings higher difficulty to the purification of the final product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Embodiment 1. ethanol purification

[0038] Take 90kg each of I-01 and I-02, and operate two batches in parallel in the following manner. 250 kg of ethanol was pumped into a 500L reactor, heated and stirred to dissolve, stirred and crystallized, filtered by rejection, and dried to obtain a yellow solid. The specific yield and purity are shown in Table 2 below:

[0039] Table 2

[0040] Numbering

[0041] Remarks: a The retention time is about 7.9min, and the relative retention time is 1.13.

Embodiment 2

[0042] Embodiment 2. dichloromethane-n-hexane purification once

[0043] Take 60kg each of the above-mentioned I-01-E1 and I-01-E2, and operate in parallel.

[0044] Specific operation: inhale dichloromethane into the reaction kettle, add the crude product, stir to dissolve, filter through 8 kg of diatomaceous earth, then pour the filtrate into the crystallization kettle, add n-hexane to precipitate Erecoxib, stir, and filter , dried to give a white solid. Concrete yield and purity are shown in Table 3 below:

[0045] table 3

[0046] Numbering

[0047] Remarks: a The retention time is about 7.9min, and the relative retention time is 1.13.

Embodiment 3

[0048] Embodiment 3. dichloromethane-normal hexane is purified twice

[0049] Take 40 kg each of I-01-E1-D1 and I-02-E1-D1 obtained from the above methylene chloride-n-hexane purification once, and operate in parallel. The specific operation steps are as in Example 2. The yield and purity are shown in Table 4 below:

[0050] Table 4

[0051] Numbering

Output (kg)

yield

Purity (HPLC)

unknown complex a

Absorbance

I-01-E1-D2

35

86.2％

99.79％

0.03％

0.128

I-02-E1-D2

36

89.6％

99.77％

0.03％

0.049

[0052] Remarks: a The retention time is about 7.9min, and the relative retention time is 1.13.

[0053] In the present invention, the testing methods and standards about related substances and absorbance are as follows:

[0054] Avoid light operation. Take 1.00g of this product, weigh it accurately, put it in a 10ml brown measuring bottle, add 8ml of dimethyl sulfoxide, heat at 60°C for 5 minutes to dissolve, ...

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PUM

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Abstract

The invention relates to an imrecoxib purifying method, which comprises: purifying an imrecoxib crude product by using a first solvent system. According to the present invention, the process is stableafter the method is subjected to scale-up; and with the method, the high-purity imrecoxib raw material meeting the pharmaceutical standard can be obtained.

Description

technical field [0001] The invention relates to a purification method of Erecoxib. technical background [0002] Erecoxib, chemical name: N-propyl-3-(4-methylphenyl)-4-(4-methylsulfonylphenyl)-2,5-dihydropyrrol-2-one, Structure is as shown in formula (I): [0003] [0004] Erecoxib is a selective cyclooxygenase-2 (COX-2) inhibitor. Studies have shown that Erecoxib is mainly metabolized by cytochrome oxidase CYP2C9 in the human body. Prior art CN1134413C, CN101386590A, etc. disclosed the preparation method of Erecoxib and its analogues but did not mention the purification. CN101774958B disclosed a preparation method of the crystal form of Erecoxib, any crystal form or amorphous The Erecoxib solid is heated and dissolved in an appropriate amount of organic solvents selected from methanol, ethanol, isopropanol or its aqueous solution, and then slowly cooled and crystallized to obtain the Erecoxib I crystal form. [0005] The color of the Erecoxib sample obtained according...

Claims

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Application Information

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IPC IPC(8): C07D207/38A61K31/4015
CPCA61K31/4015C07D207/38
Inventor 朱汉帅
Owner JIANGSU HENGRUI MEDICINE CO LTD