Novel crystal form of salt formed by etoricoxib and hydrochloric acid and preparation method of novel crystal form

A technology of etoricoxib and hydrochloric acid, which is applied in the field of new crystal forms of salts formed by etoricoxib and hydrochloric acid and its preparation, can solve problems affecting the purity and quality of drugs, incomplete removal, etc., and achieve good solubility and stability.

Inactive Publication Date: 2018-01-09
JIANGSU QINGJIANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the process of synthesizing etoricoxib, some important intermediates may affect the purity and quality of the drug due to incomplete removal
So far, there are few relevant reports about the crystal form of etoricoxib salt. In view of this, the technical problem to be solved in the present invention is to overcome the deficiencies in the prior art and provide a new salt form of etoricoxib and its preparation method , with good solubility and stability, laying the foundation for the development and application of new dosage forms

Method used

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  • Novel crystal form of salt formed by etoricoxib and hydrochloric acid and preparation method of novel crystal form
  • Novel crystal form of salt formed by etoricoxib and hydrochloric acid and preparation method of novel crystal form
  • Novel crystal form of salt formed by etoricoxib and hydrochloric acid and preparation method of novel crystal form

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Under ice bath, add etoricoxib (358mg, 1mmol) and hydrochloric acid (0.5mmol) into a 50ml Erlenmeyer flask, add 20ml of methanol, add in batches, when the solution is slightly turbid, stop adding, stir for 2 hours , placed in an explosion-proof refrigerator with a room temperature of 10 degrees, and slowly precipitated to obtain the product.

Embodiment 2

[0021] Under ice bath, add etoricoxib (350mg, 1mmol) and hydrochloric acid (1mmol) into a 50ml Erlenmeyer flask, add 20ml of methanol, add in batches, when the solution is slightly turbid, stop adding, stir for half an hour, Placed in an explosion-proof refrigerator at 0°C, slowly precipitated, filtered and dried to obtain the product.

Embodiment 3

[0022] Embodiment 3: high temperature test

[0023] Two temperature levels of 40°C and 60°C were selected for the temperature respectively. The samples were placed at 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

The invention discloses a crystal form of a salt formed by etoricoxib and hydrochloric acid and a preparation method of the crystal form and belongs to the technical fields of discovery and preparation of crystal forms of medicinal salts. The salt formed by etoricoxib and hydrochloric acid prepared in the invention is detected to be a salt formed by etoricoxib and hydrochloric acid by analysis methods such as thermogravimetry analysis (TGA), powder X-ray diffraction (P-XRD), X ray single crystal diffraction (S-XRD), differential scanning calorimetry (DSC), ultraviolet spectrum (UV), H nuclearmagnetic resonance (H-NMR) and the like. The etoricoxib is an insoluble drug, the salt formed by the etoricoxib and the hydrochloric acid is tested to have good solubility and stability in a solid preparation preparing process, and a foundation is laid for development and application of the novel crystal form of the salt.

Description

technical field [0001] The invention relates to a salt crystal formed by etoricoxib and hydrochloric acid and a preparation method thereof, in particular to a new crystal form of a salt formed by etoricoxib and hydrochloric acid and a preparation method thereof, belonging to the technical field of drug crystal form discovery and preparation. 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), molecular formula 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 ...

Claims

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Application Information

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IPC IPC(8): C07D213/61
Inventor 张勇马玉恒
Owner JIANGSU QINGJIANG PHARMA
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