Preparation method of gemfibrozil crystal form I

A technology of fibrozil crystal form and gemfibrozil, which is applied in the field of medicinal chemistry, can solve the problems of large amount of three wastes and low yield, and achieve the effects of reducing the generation of three wastes, high yield, and obvious economic benefits
CN108558654BActive Publication Date: 2021-09-07浙江精进药业有限公司
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
浙江精进药业有限公司
Publication Date
2021-09-07

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Abstract

The invention discloses a preparation method of gemfibrozil crystal form I, which comprises the following steps: 1), adding 10 g of gemfibrozil into 20-50 ml of ethanol, stirring until gemfibrozil dissolves; 2), crystallizing, selecting Either of the following methods: method 1, add 20±5ml of water dropwise to the gemfibrozil ethanol solution obtained in step 1), after the dropwise addition, cool down to 10±2°C, stir for 1.5 to 2.5 hours, and filter; method 2 . Add dropwise the gemfibrozil ethanol solution obtained in step 1) into a mixed solvent consisting of 12-15ml of water and 6ml of ethanol. After the dropwise addition, cool down to 10-20°C, stir for 1-2 hours, and filter ; 3), the filter cake obtained by filtering in step 2) was vacuum-dried at 40±5° C. for 7-8 hours to obtain Gefibrozil crystal form I. The preparation of the gemfibrozil crystal form I by the method has a high yield and can significantly reduce the environmental protection pressure of enterprises.
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Description

technical field

[0001] The invention belongs to the technical field of medicinal chemistry, and in particular relates to a preparation method of crystal form I of gemfibrozil. Background technique

[0002] Gemfibrozil (Gemfibrozil), chemical name 2,2-dimethyl-5-(2,5-dimethylphenyloxy)-pentanoic acid, the structure is as follows:

[0003]

[0004] Gemfibrozil is a clofibrate lipid-regulating drug for the treatment of hyperlipidemia, suitable for severe type IV or V hyperlipoproteinemia, coronary heart disease, type IIb hyperlipoproteinemia and other blood lipid regulating drugs invalid.

[0005] Gemfibrozil synthesis has been reported at home and abroad with a variety of technological routes, ES545970, US3674838, CN1072823 and other documents have reported synthetic methods.

[0006] There are also literature reports on the crystal form of gemfibrozil. Patent EP0462066 reports a method for preparing an amorphous form, and CN200810162023 reports a method for preparing cry...

Claims

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