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Parecoxib sodium crystalline compound and preparation method thereof

A technology of parecoxib sodium and crystal compounds, applied in the field of parecoxib sodium crystal compounds and its preparation, can solve the problems of unfavorable drug safety, easy moisture absorption, etc., and achieve suitable for large-scale production, improve moisture absorption, good fluidity

Active Publication Date: 2017-08-18
SHANDONG YUXIN PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] Parecoxib sodium in the prior art has certain defects, especially its hygroscopicity, which is easy to absorb moisture and cause hydrolysis into valdecoxib, which is not conducive to drug safety

Method used

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  • Parecoxib sodium crystalline compound and preparation method thereof
  • Parecoxib sodium crystalline compound and preparation method thereof
  • Parecoxib sodium crystalline compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] Embodiment 1, the preparation of crystal compound of the present invention

[0059] Add 100.00g of the crude product of Parecoxib Sodium into a mixed solvent composed of 500ml N,N-dimethylformamide and 100ml purified water, heat to 45°C and dissolve; after the solid is dissolved, add 5g of activated carbon and keep at 45°C decarburization at low temperature for 30 min, and filter; transfer the filtrate into a three-necked flask, add 2000 ml of ethyl acetate, transfer to cold hydrazine, control the temperature at 0°C and stir for crystallization for 4 h; filter with suction, wash with 200 ml of ethyl acetate to obtain a crystalline solid, Vacuum-dried at 50°C for 8 hours to obtain 89.98 g of parecoxib sodium monohydrate.

Embodiment 2-12

[0061]

[0062]

[0063] Further illustrate the present invention by experimental example below:

experiment example 1

[0064] Experimental example 1. Humidity test

[0065] This experimental example has investigated the hygroscopicity of the parecoxib sodium crystalline compound provided by the present invention, according to the Chinese Pharmacopoeia 2010 edition two appendix ⅪⅩJ drug hygroscopicity test guideline, the temperature of setting artificial climate box is 25 ℃, relative humidity 95%.

[0066] Table 1: Humidity test results

[0067] sample 1 2 3 4 5 6 7 8 Humidification weight gain percentage 0.081 0.088 0.086 0.087 0.091 5.35 6.78 0.397

[0068] Samples 1-5 are 5 batches of samples prepared by the preparation process of Example 1;

[0069] Sample 6-7 is the sample of commercially available parecoxib sodium raw material;

[0070] Sample 8 refers to the hemihydrate prepared by patent CN 104418819A;

[0071] As can be seen from Table 1, the parecoxib sodium crystalline compound of the present invention has no hygroscopicity, and when exposed to ...

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Abstract

The invention belongs to the technical field of medicine, and discloses a parecoxib sodium crystalline compound and a preparation method thereof. The parecoxib sodium crystalline compound is different from the prior art, and is parecoxib sodium monohydrate; an X-ray powder diffraction spectrum shown by a diffraction angle being 2 theta+ / -0.2 degrees shows characteristic diffraction peaks in positions of 2.055 degrees, 3.045 degrees, 3.727 degrees, 9.849 degrees, 11.636 degrees, 14.209 degrees, 27.418 degrees, 28.636 degrees, 30.582 degrees, 31.418 degrees, 32.436 degrees, 34.018 degrees, 35.782 degrees, 36.927 degrees and 38.618 degrees; the X-ray powder diffraction spectrum obtained through Cu-K alpha ray measurement is shown as Figure 1. The parecoxib sodium crystalline compound disclosed by the invention has the advantages that the stability is high; moisture absorption cannot easily occur in a high-humidity state; the preparation method is simple and is easy to operate; the medication safety is greatly improved; the parecoxib sodium crystalline compound is very suitable for clinical application.

Description

technical field [0001] The invention belongs to the technical field of medicine and discloses a parecoxib sodium crystal compound and a preparation method thereof. Background technique [0002] Parecoxib Sodium (Parecoxib Sodium), developed by Pfizer, is the first specific COX-2 inhibitor that can be administered intravenously (IV) and intramuscularly (IM). Cloth and Erecoxib are drugs of the same kind, used for short-term treatment of postoperative pain, and were launched in Europe in March 2002. The chemical name is: N-[[4-(5-methyl-3-phenyl-4-isoxazolyl)phenyl]sulfonyl]propionamide sodium salt, and the molecular formula is: C 19 h 17 N 2 NaO 4 S, molecular weight: 392.41. [0003] As the prodrug of valdecoxib, parecoxib sodium has high solubility and is easily hydrolyzed to valdecoxib. Although parecoxib sodium is rapidly converted into valdecoxib in the body to play a role, due to the poor water solubility of valdecoxib, if it is converted into more valdecoxib in v...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D261/08
Inventor 陈雨朱绪辉王平耿强
Owner SHANDONG YUXIN PHARMA CO LTD