Method for preparing etoricoxib crystal form V

A technology of etoricoxib and demethyst, which is applied in the field of medicinal chemistry, can solve the problems that the preparation method of crystal form V is not mentioned, and it is difficult to obtain crystal form V repeatedly.

Active Publication Date: 2017-08-18
四川尚锐生物医药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is no mention of the preparation method of crystal form V
[0008] The above-mentioned existing literature has carried out many studies on the crystal form of etoricoxib, but there are few references to the prepa...

Method used

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  • Method for preparing etoricoxib crystal form V
  • Method for preparing etoricoxib crystal form V
  • Method for preparing etoricoxib crystal form V

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Add 50 g of etoricoxib crude product into 250 mL of 5 times the volume of toluene, heat to 70 ° C to dissolve, keep the temperature at 60 ° C, add a little acetic acid (the amount is about 0.1% of the etoricoxib molar mass), stir for about 0.5 h, slowly Cool down and crystallize, filter, and dry to obtain etoricoxib Form V 45.3g. Measured melting point: 134.5-138.3°C.

[0025] Adopt Cu target X-ray powder diffractometer to measure the X-ray powder diffraction pattern (XRD figure) of gained crystal form, see figure 1 , the 2θ value and relative intensity I% of its characteristic absorption peak are shown in Table 1.

[0026] Table 1 XRPD determines the 2θ value and relative intensity I% of etoricoxib polymorph absorption peak

[0027]

[0028]

[0029] Adopt TGA and DSC 2 LF1100 / 155 test instrument (TGA DSC 40-350 ℃ 10 ℃ / min) to carry out differential scanning calorimetric analysis DSC and thermogravimetric analysis TGA to the gained crystal form, the result sees...

Embodiment 2

[0031] Add 500g of crude etoricoxib to 2500mL of isopropyl acetate with 5 times the volume, heat to 70°C to dissolve, keep the temperature between 68-70°C and add a little acetic acid (the amount is about 0.5% of the molar mass of etoricoxib) , stirred for about 0.4-0.5h, slowly cooled down to crystallize, filtered, and dried to obtain etoricoxib Form V 467.6g. Measured melting point: 135.5-137.4°C.

Embodiment 3

[0033] Add 45g of etoricoxib crude product into 420mL of 7 times the volume of ethyl acetate, heat to 65°C to dissolve, keep the temperature at about 65°C, add a little propionic acid (the amount is about 0.01% of the molar mass of etoricoxib), and stir for about After 0.4-0.6h, the temperature was slowly lowered for crystallization, filtered, and dried to obtain 43.5g of etoricoxib Form V. Measured melting point: 134.8-138.0°C.

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Abstract

The invention discloses a method for preparing an etoricoxib crystal form V. The method comprises the steps that etoricoxib is dissolved in an appropriate solvent, little acid is added to induce crystallization, and filtering and drying are performed to obtain the etoricoxib crystal form V. The method is simple in operation, good in reproducibility, high in yield and suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of medicinal chemistry, and specifically relates to a method for preparing etoricoxib crystal form V, a pharmaceutical composition and a medical application. Background technique [0002] Etoricoxib is a selective inhibitor of cyclooxygenase-2, which has anti-inflammatory, antipyretic and analgesic effects. Its chemical structure is as follows. [0003] [0004] At present, the film-coated tablets of etoricoxib have been marketed in many countries such as the United Kingdom, Spain, Australia, and China, and are mainly used as non-steroidal anti-inflammatory drugs in clinical practice. [0005] The crystal form of etoricoxib has a great influence on the properties of the drug. Patent WO2001092230A1 discloses the properties and preparation methods of eight crystal forms of etoricoxib, including crystal form I, crystal form II, crystal form III, crystal form IV, Form V, hemihydrate, sesquihydrate and amorphous state,...

Claims

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Application Information

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IPC IPC(8): C07D213/61A61K31/4418A61P29/00A61P25/04
CPCC07B2200/13C07D213/61
Inventor 刘超常繁彭显峰戴萍
Owner 四川尚锐生物医药有限公司
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