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Novel crystal form of salts prepared from etoricoxib and p-toluene sulfonic acid and preparation method thereof

A technology of p-toluenesulfonic acid and etoricoxib, which is applied in the fields of sulfonate preparation, organic chemistry methods, organic chemistry, etc.

Pending Publication Date: 2019-08-20
BENGBU COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But so far, there has not been any report on the new crystal form of etoricoxib synthesized with p-toluenesulfonic acid as a reactant. In view of this, the present invention provides a salt form and preparation method of etoricoxib, which has Good solubility and stability, and the development of new salt forms have laid the foundation for the development and application of new dosage forms

Method used

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  • Novel crystal form of salts prepared from etoricoxib and p-toluene sulfonic acid and preparation method thereof
  • Novel crystal form of salts prepared from etoricoxib and p-toluene sulfonic acid and preparation method thereof
  • Novel crystal form of salts prepared from etoricoxib and p-toluene sulfonic acid and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Example 1 Preparation of etoricoxib and p-toluenesulfonic acid to form a salt

[0020] Under ice-cooling, etoricoxib (358mg, 1mmol) and p-toluenesulfonic acid (0.8mmol) were added in a 50ml Erlenmeyer flask, and 20ml of methanol was added in batches, and after stirring for half an hour, stop stirring when the solution was slightly turbid. , placed in an explosion-proof refrigerator at 10°C, slowly precipitated, filtered to remove excess solvent, washed, and vacuum-dried to obtain the product.

Embodiment 2

[0021] Example 2 Preparation of etoricoxib and p-toluenesulfonic acid to form a salt

[0022] Under ice bath, add etoricoxib (350mg, 1mmol) and p-toluenesulfonic acid (1.2mmol) into a 50ml Erlenmeyer flask, add 20ml methanol in batches, stop adding when the solution is slightly turbid, and stir for half an hour Finally, place it in an explosion-proof refrigerator at 0°C for slow precipitation, filter to remove excess solvent, wash, and vacuum-dry to obtain the product.

Embodiment 3

[0023] Embodiment 3 carries out high temperature test test to embodiment 1 gained salt crystal product

[0024] Two temperature levels of 40°C and 60°C were selected for the temperature respectively: the salt crystal sample obtained in Example 1 was placed at 60°C for 10 days, and samples were taken on the 5th and 10th days, and tested according to the key stability inspection items; if 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% decrease 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

The invention discloses a crystal form of pharmaceutical salts, which are prepared from etoricoxib and p-toluene sulfonic acid and used as a selective COX-2 inhibitor and a preparation method thereof,and belongs to the technical field of novel pharmaceutical salt preparation. The salts prepared from etoricoxib and p-toluene sulfonic acid are detected by following analysis methods: thermogravimetric analysis (TGA), X-ray powder diffraction (P-XRD), X-ray single crystal diffraction (S-XRD), differential scanning calorimetry (DSC), ultraviolet spectrum (UV), H-NMR, and the like. Etoricoxib is difficult to dissolve, the salts prepared from etoricoxib and p-toluene sulfonic acid are applied to solid preparations, the solubility and stability are good, and the development of novel crystal formsof the salts lays a foundation for the development and application of novel dosage forms.

Description

technical field [0001] The invention belongs to the technical field of preparation of new salts of medicines, and in particular relates to a new crystal form of salts formed by etoricoxib and p-toluenesulfonic acid and a preparation method thereof. Background technique [0002] Etoricoxib is a highly selective cyclooxygenase-2 (COX-2) inhibitor drug, the English name is Etoricoxib, the chemical name is [5-chloro-2-(6-methylpyridin-3 base)-3 -(4-Methylsulfonylphenyl)pyridine (5-Chloro-3-(4-methanesulfonyl-phenyl)-6'-methyl-[2,3']bipyridinyl), the molecular formula is C 18 h 15 ClN 2 o 2 S. [0003] Etoricoxib is used in the treatment of osteoarthritis (OA), rheumatoid arthritis and acute gouty arthritis. Etoricoxib is an analgesic drug with improved performance compared with traditional non-steroidal anti-inflammatory drugs (NSAIDs), and it is the only coxib drug that has been proven effective in the treatment of acute gouty arthritis. Other indications currently approv...

Claims

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Application Information

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IPC IPC(8): C07D213/61C07C303/32C07C309/30
CPCC07D213/61C07C303/32C07B2200/13C07C309/30
Inventor 冯超马玉恒郭晶晶
Owner BENGBU COLLEGE
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