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Purification method of etoricoxib

A purification method and etoricoxib technology, applied in the direction of organic chemistry, etc., can solve the problems such as difficult to solve the color impurities of etoricoxib bulk drug

Pending Publication Date: 2021-02-05
四川尚锐生物医药有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This also shows from the other hand that the etoricoxib raw material drug does have the problem of color impurities that are difficult to solve

Method used

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  • Purification method of etoricoxib
  • Purification method of etoricoxib
  • Purification method of etoricoxib

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Weigh 20.0 g of etoricoxib crude product to be purified (HPLC purity 99.661%, single largest impurity 0.282%), add 50 mL of acetone, stir at room temperature, the solid gradually dissolves, and then the system slowly becomes turbid again, cool down to - Crystallize at 5-0°C, filter, and dry. After crystallization, a white crystalline powder is obtained (see Figure 5 ) 16.1 g. The color of the solution prepared according to the requirements is between yellow or yellow-green No. 0.5 and No. 1 standard colorimetric solution (Chinese Pharmacopoeia 2015 Edition Four General Rules 0901 First Method), and its absorbance is 0.080. Yield 80.5%. Detected by HPLC, the purity is 99.994%, and the single largest impurity is 0.006% (see Figure 6 ).

Embodiment 2

[0052] Weigh 16.0 g of the crude etoricoxib to be purified (HPLC purity 99.661%, single largest impurity 0.282%), add 40 mL of acetone, stir at room temperature, the solid gradually dissolves, then the system slowly becomes turbid again, and the temperature is lowered to 0 Crystallize at ~5°C, add 40ml of water, filter, and dry. After crystallization of the obtained sample, 13.3g of white crystalline powder is obtained. The color of the solution prepared according to the requirements is between yellow or yellow-green No. 0.5 and No. 1 standard colorimetric solution (Chinese Pharmacopoeia 2015 Edition Four General Rules 0901 First Method), and its absorbance is 0.112. Yield 83.1%. Detected by HPLC, the purity is 99.983%, and the single largest impurity is 0.017% (see Figure 7 ).

Embodiment 3

[0054] Weigh 36.3 g of the crude etoricoxib to be purified (HPLC purity 99.750%, single largest impurity 0.222%), add 108 mL of methyl isobutyl ketone, stir at room temperature, the solid gradually dissolves, and then the system slowly becomes turbid , cooled to 5-10° C. for crystallization, added 108 ml of water, filtered, and dried. After crystallization of the obtained sample, 30.5 g of white crystalline powder was obtained. The color of the solution prepared according to the requirements is between yellow or yellow-green No. 0.5 and No. 1 standard colorimetric solution (Chinese Pharmacopoeia 2015 Edition Four General Rules 0901 First Method), and its absorbance is 0.105. Yield 84.0%. As detected by HPLC, the purity is 99.974%, and the largest single impurity is 0.018%.

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Abstract

The invention discloses a purification method of etoricoxib, wherein the method comprises the steps: adding a crude etoricoxib product to be purified into a ketone solvent at room temperature, addingor not adding a poor solvent after a solid is dissolved and becomes turbid, cooling to crystallize, filtering, drying, carrying out further crystal transformation on the obtained sample, and thus obtaining the high-purity final product. The method is suitable for industrial mass production, conditions are mild, operation is easy, and the tedious process steps of salifying and dissociation in the subsequent purification step are avoided.

Description

technical field [0001] The invention belongs to the field of medicinal chemistry, and in particular relates to a purification method of etoricoxib. 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] Etoricoxib has been marketed in 84 countries and regions including the UK, Spain, Australia, and China in the form of film-coated tablets, and is mainly used clinically as a non-steroidal anti-inflammatory drug. The American College of Rheumatology guidelines for the diagnosis and treatment of gout recommend etoricoxib for the treatment of acute gouty arthritis. The guidelines for the diagnosis and treatment of osteoarthritis in my country and the orthopedic pain management expert opinion of the Orthopedic Branch of the Chinese Medical Association also recommend etoricoxib for patients with gastrointestinal risk. [0005]...

Claims

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Application Information

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IPC IPC(8): C07D213/61
CPCC07D213/61
Inventor 刘超吴昆杨以建叶子峥唐燕彭显峰戴萍
Owner 四川尚锐生物医药有限公司
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