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A kind of equipment and method for purifying parecoxib sodium

A parecoxib sodium and purification method technology, which is applied in the field of pharmaceutical technology and equipment, can solve the problems that the crystallization rate affects the crystal refining effect, the solubility of parecoxib sodium decreases, and the filter press process is blocked by filtration equipment, etc., so as to achieve easy implementation and promotion, ensuring the stability of the crystallization rate, and solving the effects of easy clogging

Active Publication Date: 2022-05-20
JIANGSU SINOBIOPHARMA
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AI Technical Summary

Problems solved by technology

Parecoxib sodium is slightly soluble in ethanol at room temperature, and its solubility increases rapidly as the temperature rises. This characteristic leads to the following defects in the ethanol recrystallization process of parecoxib sodium: When using 2 times the volume of absolute ethanol, it can be completely dissolved. As a result, in actual production, the amount of solvent used in the recrystallization process of parecoxib sodium is relatively small, and it is difficult to match the equipment when the crystal is filtered into the clean area. ;②During the filter press process, the solubility of parecoxib sodium will decrease rapidly due to the temperature drop, and the possibility of solid precipitation in advance is high. If the crystals are precipitated in the filter in advance, it will cause blockage of the filter equipment and affect the filter press process. At the same time, if the crystallization rate is too fast, it will also affect the refining effect of the crystal.

Method used

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  • A kind of equipment and method for purifying parecoxib sodium

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Embodiment Construction

[0021] The ethanol recrystallization refining method of traditional parecoxib sodium takes the crude product of parecoxib sodium as a raw material, recrystallizes through absolute ethanol, and obtains the refined product of parecoxib sodium through separation and drying. The method specifically includes the following steps:

[0022] 1) Feeding: put the crude product of parecoxib sodium and 2-10 times the volume of absolute ethanol into the reaction kettle, stir and heat up to 70±2°C, keep stirring until the solid dissolves completely, and obtain the reaction solution;

[0023] 2) Pressure filtration: Press filter the completely dissolved reaction liquid into the reaction kettle in the clean area while it is hot;

[0024] 3) Crystallization: Slowly lower the temperature of the reaction solution to 20-25°C, heat and stir for 2 hours to obtain a filter cake;

[0025] 4) Centrifugation: wash the filter cake with absolute ethanol and centrifuge until dry and collect the filter cake...

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Abstract

The invention proposes a device and method for purifying parecoxib sodium. The pipeline, the second pipeline and the third pipeline; wherein the bottom of the main reactor is connected to the liquid distributor through the first pipeline, the bottom of the auxiliary reactor is connected to the liquid distributor through the second pipeline, and the bottom of the crystallization kettle is provided with The filter is connected to the liquid distributor through the third pipeline; the high-pressure nitrogen tank is connected to the top of the main reactor and the auxiliary reactor through the gas transmission pipeline, and the bottom of the liquid distributor is connected to the liquid storage tank through the infusion pipeline. On the basis of not changing the existing parecoxib sodium crystallization solvent and crystallization conditions, the invention can effectively ensure that the product is a medicinal crystal form, ensure that the temperature is stable in the whole reaction process, avoid the product from precipitation in the pressure filtration process, and at the same time the crystallization rate It is stable and can effectively ensure the refining effect of crystals.

Description

technical field [0001] The invention relates to equipment and a method for purifying parecoxib sodium, belonging to the technical field of pharmaceutical technology and equipment. Background technique [0002] Parecoxib sodium is a selective COX-2 inhibitor that can be injected intravenously or intramuscularly for short-term treatment of postoperative pain. Parecoxib sodium is a non-steroidal anti-inflammatory drug, an amide precursor compound of the highly selective COX-2 inhibitor valdecoxib, which can be rapidly hydrolyzed into valdecoxib by liver carboxylesterase after intravenous injection, It exerts anti-inflammatory and analgesic effects by specifically inhibiting COX-2 and blocking the synthesis of prostaglandins from arachidonic acid. [0003] In the current production process of parecoxib sodium, its purification methods include ethanol recrystallization method, ethanol dissolving and adding n-heptane crystallization method, n-heptane suspension heating method, et...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J19/18B01D9/00C07D261/08
CPCB01J19/18B01D9/00C07D261/08Y02P20/10
Inventor 吴邵嘉黄乐群
Owner JIANGSU SINOBIOPHARMA
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