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A crystal form of a salt formed from phthalic acid and etoricoxib and a preparing method thereof

A technology of phthalic acid and etoricoxib is applied in the field of crystal form and preparation of salts, and the preparation of co-crystals of pharmaceutical compounds, and can solve the problems of low utilization rate and the like

Inactive Publication Date: 2018-02-16
JIANGSU QINGJIANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Currently, only 10 salt-forming acidic coordinating molecules are used more than 1 %, and basic coordinating molecules are used even less

Method used

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  • A crystal form of a salt formed from phthalic acid and etoricoxib and a preparing method thereof
  • A crystal form of a salt formed from phthalic acid and etoricoxib and a preparing method thereof
  • A crystal form of a salt formed from phthalic acid and etoricoxib and a preparing method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] At room temperature, accurately weigh the etoricoxib raw material (359mg, 1mmol) into a 50ml beaker, add phthalic acid (166mg, 1mmol), add anhydrous methanol dropwise under ultrasonication until it is completely dissolved, continue Sonicate for 5min and filter with filter paper.

[0021] Transfer the filtrate to a 50ml beaker, place the 50ml beaker in a large beaker filled with purified water, and conduct vacuum evaporation and crystallization at room temperature (vacuum degree -0.05MP). After about 72-96 hours, a large number of transparent massive crystals precipitated, filtered, and the filter cake was washed with cold methanol to obtain the desired salt crystals.

Embodiment 2

[0023] At room temperature, accurately weigh the etoricoxib raw material (359mg, 1mmol) into a 50ml beaker, add phthalic acid (166mg, 1mmol), add anhydrous methanol dropwise under ultrasonication until it is completely dissolved, continue Sonicate for 5min and filter with filter paper.

[0024] Transfer the filtrate to a 50ml beaker, place the 50ml beaker in a large beaker filled with purified water, and conduct vacuum evaporation and crystallization at 60°C (vacuum degree -0.08MP). After about 48-72 hours, a large number of transparent blocky crystals precipitated, filtered, and the filter cake was washed with cold methanol to obtain the desired salt crystals.

Embodiment 3

[0025] Embodiment 3: high temperature test

[0026] Two temperature levels of 40°C and 60°C were selected for the temperature respectively. The samples were placed at a temperature of 60°C for 10 days, and samples were taken on the 5th and 10th days, and tested according to the key items of stability investigation. If there is no obvious change in the sample, the test at 40°C will not be carried out; if the sample has obvious changes (such as a 5% drop in content, a large change in appearance and color if the identification is not obvious, etc.), the test must be carried out in the same way at 40°C.

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Abstract

A salt formed from phthalic acid and etoricoxib, which is prepared by the invention, is proved to be a salt which is formed from the phthalic acid and the etoricoxib and in which the mole ratio of thephthalic acid to the etoricoxib is 1:1 through thermogravimetric analysis (TGA), proton nuclear magnetic resonance (H-NMR), X-ray powder diffraction (P-XRD), ultraviolet (UV), X-ray diffraction of single crystal (S-XRD), differential scanning calorimetry (DSC), and other analysis methods. Compared with other solid states of the etoricoxib, a cocrystal of the phthalic acid and the etoricoxib has potential improvements in solubility, bioactivity and physical stability, and can improve medicine hygroscopicity, chemical stability, and the like.

Description

technical field [0001] The invention relates to the preparation of a co-crystal of a pharmaceutical compound, in particular to the crystal form of a salt formed by etoricoxib and phthalic acid and a preparation method thereof, belonging to the field of synthesis of pharmaceutical intermediates. Background technique [0002] Etoricoxib, trade name Arcoxia, chemical name: 5-chloro-6'-methyl-3-[4-(methylsulfonyl)phenyl]-2,3'-bipyridine , is a highly selective cyclooxygenase-2 (COX-2) inhibitor developed by Merck. Etoricoxib has a unique chemical structure, that is, a methylsulfonyl group. The introduction of this group not only increases the selectivity of the drug to COX-2, but also does not produce cross-allergic reactions with sulfa drugs. Etoricoxib was first approved for marketing in the UK in 2002, followed by countries and regions including the European Union, Asia Pacific, Australia, and Latin America. By the end of 2013, it had been approved for marketing in 97 countr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/61
Inventor 郑强李新辈黎志明陈世龙王海珊
Owner JIANGSU QINGJIANG PHARMA
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