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Gemfibrozil polymorphism and preparation method thereof

A felozil crystal form and a technology for gemfibrozil, which is applied in the field of medicinal chemistry, can solve the problems of difficulty in storage, poor amorphous stability of gemfibrozil, etc., and achieve the effects of no reduction in drug content, good stability and easy production.

Inactive Publication Date: 2009-10-14
浙江精进药业有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The present invention aims at the poor amorphous stability of gemfibrozil in the prior art and the problem of difficulty in preservation, and provides a polymorphic preparation method of gemfibrozil, Gemfibrozil is dissolved in a certain amount of alcohol, ketone, ester, ether solvent, crystallized, filtered, and dried to obtain gemfibrozil crystal form I, which has good stability and is convenient for production, transportation and storage

Method used

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  • Gemfibrozil polymorphism and preparation method thereof
  • Gemfibrozil polymorphism and preparation method thereof
  • Gemfibrozil polymorphism and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0019] Add 10 g of gemfibrozil to a mixed solvent composed of 5 mL of acetone and 2 mL of cyclohexane, heat (about 50 ° C) to reflux, stir until completely dissolved, transfer the solution to an ice-water bath (0 to 5 ° C) for crystallization, The solid was separated by filtration and dried in vacuum at 40° C. for 8 hours to obtain gemfibrozil in crystal form I.

Embodiment 2

[0021] Add 10g of gemfibrozil to 5mL of petroleum ether, heat (about 50°C) to reflux, stir until completely dissolved, crystallize in an ice-water bath at 0-5°C, separate by filtration to obtain a solid, and dry in vacuum at 40°C for 8 hours , to obtain I crystal form gemfibrozil.

Embodiment 3

[0023] Add 10g of gemfibrozil to a mixed solvent consisting of 2mL of ethanol and 10mL of cyclohexane, heat (about 50°C) to reflux, stir until completely dissolved, crystallize in an ice-water bath at 0-5°C, and separate by filtration to obtain a solid. °C and dried under vacuum for 8 hours to obtain crystal form I of gemfibrozil.

[0024] The X-ray powder diffraction pattern (XRD) of the gemfibrozil crystal form I of above-mentioned embodiment 1-3, see figure 1 , X-ray diffraction patterns of gemfibrozil crystals at 2θ (°, ±0.2) 6.32°, 11.52°, 11.89°, 12.69°, 13.45°, 13.83°, 15.02°, 16.65°, 17.14°, 17.39°, 17.99 °, 17.27°, 18.78, 19.13°, 19.79°, 21.95°, 23.27°, 24.23°, 25.12°, 26.92°, 34.94°, showing characteristic diffraction peaks. Infrared absorption spectrum wavenumber in potassium bromide (cm -1 ) for: 1705, 1509, 1472, 1402, 1285, 1270, 1212, 1158, 1128, 1047, 940, 802cm -1 wait, see attached figure 2 . There is an endothermic peak at 60.8°C in the differential th...

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Abstract

The invention relates to Gemfibrozil polymorphism and a preparation method thereof. The preparation method comprises the following steps: the Gemfibrozil is dissolved in a certain amount of a solvent with alcohol, ketone, ester and ether, and crystallized, filtered and dried to form a Gemfibrozil crystal form I, and an X-ray diffraction pattern of the crystal form I shows characteristic diffraction peaks at 2 theta (degrees, + / -0.2) 6.32 degrees, 11.52 degrees, 11.89 degrees, 12.69 degrees, 13.45 degrees, 13.83 degrees, 15.02 degrees, 16.65 degrees, 17.14 degrees, 17.39 degrees, 17.99 degrees, 17.27 degrees, 18.78 degrees, 19.13 degrees, 19.79 degrees, 21.95 degrees, 23.27 degrees, 24.23 degrees, 25.12 degrees, 26.92 degrees and 34.94 degrees. The Gemfibrozil polymorphism has the advantages of simple process, good stability of the crystal forms, and convenient production, transport and storage, being capable of being stored at normal temperature for more than 2 years without change, no decrease of drug content and completely meeting drug requirements.

Description

technical field [0001] The invention belongs to the technical field of medicinal chemistry. The invention relates to a preparation method of a polymorphic form of gemfibrozil, in particular to a crystal form I of gemfibrozil and a preparation method thereof. Background technique [0002] The chemical name of Gemfibrozil is 2,2-dimethyl-5-(2,5-dimethylphenyloxy)-pentanoic acid, and the English name is 5-(2,5-dimethylphenoxy)-2. 2-dimethylpentanoic acid, the structural formula is as follows: [0003] [0004] Gemfibrozil is a new blood lipid-lowering drug that was launched in the United States in 1982. It overcomes the severe toxic and side effects of the previous blood lipid-lowering drug clofibrate on the liver, retains its effective effect, and is used to prevent arteriosclerosis and help reduce the risk of myocardial infarction. Incidence rate, after oral administration, the gastrointestinal tract absorbs well and can be taken for a long time, so it is welcomed by pat...

Claims

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Application Information

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IPC IPC(8): C07C59/13C07C51/43A61P3/06
Inventor 钱绍军赵金浩王晖胡秀荣
Owner 浙江精进药业有限公司
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