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Preparation method of Etoricoxib crystal form V

A technology based on Etoxicoxi and Oxime, which is applied in the chemical and pharmaceutical fields, can solve problems such as uncontrollable conditions and unquantifiable parameters, and achieve the effects of stable yield, low cost and high process stability

Pending Publication Date: 2018-06-29
HAINAN SIMCERE PHARMA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The present invention improves the process in the existing method described in the background technology, and solves the technical problems in the prior art that some conditions are uncontrollable, parameters cannot be quantified, etc., resulting in the inability to obtain crystal form V stably, and the yield is too high. Low phenomenon, a new preparation method of V crystal form is proposed, the process stability is high, and the parameters are clear, the operation is controllable, the reproducibility is high, and the yield is significantly improved, which is more suitable for industrial production and has high economic benefits

Method used

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  • Preparation method of Etoricoxib crystal form V
  • Preparation method of Etoricoxib crystal form V
  • Preparation method of Etoricoxib crystal form V

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Embodiment 1 (preparation of etoricoxib V crystal form)

[0030] In a dry 100ml reaction bottle, add 10g of etoricoxib free base, then add 60ml of methanol, heat up to 65°C, stir, after it is completely dissolved, turn off the heating, let it cool down naturally, after cooling down to room temperature, use an ice water bath After cooling, the internal temperature was lowered to 6°C. At this temperature, it was stirred for 2 hours, filtered, and dried in vacuum (40°C). After drying, 9.21 g of etoricoxib V crystal form samples were obtained, with a yield of 92.1%. XRPD pattern see figure 1 .

Embodiment 2

[0031] Embodiment 2 (preparation of etoricoxib V crystal form)

[0032] In a dry 100ml reaction bottle, add 10.16g of etoricoxib free base, then add 80ml of ethanol, heat up to 60°C, stir, and after it is completely dissolved, turn off the heating and let it cool down naturally. Cool in a water bath to lower the internal temperature to 2°C. At this temperature, stir for 3 hours, filter, and vacuum-dry (40°C). After drying, 9.32g of etoricoxib V crystal form sample was obtained, with a yield of 91.7%. XRPD pattern see figure 2 .

Embodiment 3

[0033] Embodiment 3 (preparation of etoricoxib V crystal form)

[0034] In a dry 100ml reaction bottle, add 9.86g of etoricoxib free base, then add 80ml of methanol, heat up to 55°C, stir, and after it is completely dissolved, add 160ml of isopropyl ether, turn off the heating, let it cool down naturally, After reaching room temperature, cool with an ice-water bath to reduce the internal temperature to 6°C. At this temperature, stir for 2 hours, filter, and vacuum-dry (40°C). After drying, 9.15g of etoricoxib V crystal form samples were obtained. 92.8%. XRPD pattern see image 3 .

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Abstract

The invention relates to a preparation method of an Etoricoxib crystal form V, in particular to an Etoricoxib crystal form V product prepared from Etoricoxib free alkali monomer. The method is feasible and controllable, simple to operate and low in cost, adopts an organic solvent with lower toxicity, effectively avoids environment pollution, is high in technical repeatability and stable in yield,can obtain pure V crystal form samples, ensures that the yield reaches greater than 90 percent, is more suitable for industrial production of Etoricoxib crystal form V, and has high economic benefit.

Description

technical field [0001] The present invention relates to the field of chemical industry and pharmacy, more specifically, relates to a preparation method of etoricoxib crystal form V. Background technique [0002] The phenomenon that the same element or compound forms crystals with completely different structures, shapes, and physical properties under different conditions is called polymorphism. Polymorphism exists widely in organic medicines. The crystallization of polymorphic medicines mostly belongs to molecular lattice, and different crystal forms are produced with different process conditions. Due to the difference in the type and purity of the crystal form of the same drug, there may be significant differences in the physical properties (such as solubility, dissolution rate, melting point, etc.) and stability (crystal form and chemical stability) of the drug, thus affecting the safety of the drug. , Effectiveness has an impact. [0003] For raw materials with polymorph...

Claims

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Application Information

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IPC IPC(8): C07D213/61
CPCC07D213/61C07B2200/13
Inventor 李瑞邹洋洋
Owner HAINAN SIMCERE PHARMA CO LTD
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