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Preparation method of etoricoxib crystal form

A technology of etoricoxib and crystal form, applied in the field of preparation of etoricoxib V crystal, can solve the problems of poor stability, low yield, low purity and the like, and achieves lower unit price of raw materials, high yield and good process reproducibility Effect

Active Publication Date: 2018-05-25
KUNMING JIDA PHARMA
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] In order to overcome the disadvantages of poor stability, low yield and low purity of the preparation process of etoricoxib in the prior art for the preparation of crystal form V, the object of the present invention is to provide a kind of etoricoxib with good repeatability, stability, high yield and high purity. Preparation method of etoricoxib V crystal form suitable for industrial scale-up production

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  • Preparation method of etoricoxib crystal form
  • Preparation method of etoricoxib crystal form
  • Preparation method of etoricoxib crystal form

Examples

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Embodiment 1

[0029] Embodiment 1: comparative embodiment, do not add crystal seed crystallization situation

[0030] Add 5g of etoricoxib and 15ml of isopropyl acetate into the three-neck flask, heat to 75°C to dissolve the solid completely, keep stirring at this temperature (75°C) for 1 hour, then slowly cool down to room temperature, stir for 2 hours, and filter. The obtained solid was air-dried at 60°C for 12 hours to obtain 4.04 g of crystal form V etoricoxib with a purity of 99.0%, a yield of 80.8%, and a specific impurity of ET-IMP-409 of 0.199%. See the attachment for the liquid phase determination spectrum of the finished product figure 1 .

Embodiment 2

[0031] Example 2: Preparation of V crystal form etoricoxib

[0032] Add 5g etoricoxib and 15ml isopropyl acetate into the three-necked flask, heat to 75°C to dissolve the solid completely, add 0.25g (5%) etoricoxib crystal form V seed crystal at this temperature (75°C), Insulated and stirred for 1h, then cooled to room temperature at a cooling rate of 10°C / h, stirred for 2h, filtered, and the resulting solid was air-dried at 60°C for 12h to obtain 4.64g of crystal form V etoricoxib with a purity of 99.86% and a yield of 92.8%. The specific impurity ET-IMP-409 is 0.063%, and the liquid phase determination spectrum of the finished product purity is shown in the attachment figure 2 , see the attached crystal form diffraction pattern of the finished product image 3 .

Embodiment 3

[0033] Example 3: Preparation of V crystal form etoricoxib

[0034] Add 5g etoricoxib and 15ml isopropyl acetate into the three-neck flask, heat to 75°C to dissolve the solid completely, add 0.15g (3%) etoricoxib crystal form V seed crystal at this temperature (75°C), Insulated and stirred for 1 hour, then cooled to room temperature at a cooling rate of 20°C / h, stirred for 2 hours, filtered, and the resulting solid was air-dried at 60°C for 12 hours to obtain 4.61 g of crystal form V etoricoxib with a purity of 99.95% and a yield of 92.2%.

[0035] Example 3: Preparation of V crystal form etoricoxib

[0036] Add 5g of etoricoxib and 15ml of isopropyl acetate into the three-neck flask, heat to 75°C to dissolve the solid completely, add 0.15g (3%) etoricoxib crystal form V seed crystal at 72°C, keep stirring for 1h, Afterwards, the temperature was lowered to room temperature at a cooling rate of 5°C / h, stirred for 2h, filtered, and the obtained solid was air-dried at 60°C for 1...

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Abstract

The invention relates to a preparation method of a V-shaped etoricoxib crystal form. The method comprises the following steps: etoricoxib is added to an organic solvent, heating is performed to fullydissolve solids, the weight percentage of etoricoxib added to the solution is 10% or lower of the V-shaped crystal form seed crystal, heat-preservation stirring is performed, the temperature is reduced to room temperature at a rate of 20 DEG C or lower per hour, stirring is performed, the crystal is filtered, and the crystal form is obtained. The preparation method of the etoricoxib V-shaped crystal form has the advantages of high yield, stable process and good reproducibility, impurities ET-IMP-409 can be removed to the greatest extent in the crystallization process, purity of the raw materials is relatively high, and the additional purification step is not required.

Description

technical field [0001] The invention belongs to the field of medicine and relates to a preparation method of etoricoxib V crystal. Background technique [0002] Etoricoxib (Etoricoxib), chemical name: 5-chloro-3-(4-methylsulfonylphenyl)-6-methyl-[2,3]bipyridine, structural formula is as follows: [0003] [0004] Etoricoxib is a highly selective COX-2 inhibitor, which exerts antipyretic, analgesic and anti-inflammatory effects by inhibiting COX and reducing the production of prostaglandin (PG) and thromboxane. It can be used for rheumatoid arthritis, OA chronic low back pain, and postoperative toothache. It has pain-relieving and anti-inflammatory effects, and has no adverse reactions such as gastrointestinal reactions caused by non-selective COX-1. [0005] Etoricoxib was first launched in Mexico, the United Kingdom, and Brazil in 2002, followed by countries and regions including the European Union, Asia-Pacific, Australia, and Latin America. By the end of 2013, it had ...

Claims

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Application Information

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IPC IPC(8): C07D213/61
CPCC07D213/61C07B2200/13
Inventor 王亮张朴永郭雷雷王立江张云
Owner KUNMING JIDA PHARMA
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