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Preparation method of gemfibrozil crystal I

A gemfibrozil and Rozier crystal form technology, applied in the field of medicinal chemistry, can solve the problems of low yield and large amount of three wastes, and achieve the effects of high yield, reduction of three wastes, and obvious economic benefits

Active Publication Date: 2018-09-21
浙江精进药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method needs to be crystallized in an ice-water bath at 0-5°C, and solvents such as ketones and alcohols are used. The yield of this method is low (the yield is about 60-70%), and a large amount of three wastes is produced.

Method used

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  • Preparation method of gemfibrozil crystal I
  • Preparation method of gemfibrozil crystal I
  • Preparation method of gemfibrozil crystal I

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Embodiment 1, a preparation method of gemfibrozil crystal form I:

[0027] Take 10g of gemfibrozil and add it to 50ml of ethanol, heat up to 30°C and stir until the gemfibrozil dissolves to obtain the gemfibrozil ethanol solution;

[0028] Slowly add 20ml of water to gemfibrozil ethanol solution (dropping time is 60-90 minutes), during the dropping process, solids will be precipitated, then lower the temperature to 10°C, stir for 2 hours, filter to obtain solids, 40°C After vacuum drying for 7-8 hours, 8.1 g of gemfibrozil crystal form was obtained, with a yield of 81%.

Embodiment 2

[0029] Embodiment 2, a preparation method of gemfibrozil crystal form I:

[0030] Take 10g of gemfibrozil and add it to 25ml of ethanol, heat up to 40°C and stir until the gemfibrozil dissolves to obtain the gemfibrozil ethanol solution;

[0031] Slowly add the gemfibrozil ethanol solution obtained dropwise (dropping time is 60 to 90 minutes) into a solution composed of 15ml of water and 6ml of ethanol. After the dropwise addition is completed, cool down to 10°C, stir for 2 hours, and filter. The obtained solid was vacuum-dried at 40° C. for 7 to 8 hours to obtain 8.5 g of gemfibrozil crystal form I, with a yield of 85%.

[0032] Remarks: The filtrate obtained by filtering is concentrated in a conventional manner, and the concentrated substrate is discarded to obtain an ethanol-water solution, which is prepared according to the ethanol-water solution ratio (1:2.5) described in Example 2 above, so as to realize recycling (recycling The number of times is at least 5 times), and...

Embodiment 3

[0034] Take 10g of gemfibrozil and add it to 20ml of ethanol, heat up to 50°C and stir until the gemfibrozil dissolves to obtain the gemfibrozil ethanol solution;

[0035] Slowly add the gemfibrozil ethanol solution obtained dropwise (dropping time is 60 to 90 minutes) into a solution composed of 12ml of water and 6ml of ethanol. After the dropwise addition is completed, cool down to 20°C, stir for 1 hour, and filter. The obtained solid was vacuum-dried at 40° C. for 7 to 8 hours to obtain 8.7 g of gemfibrozil crystal form I, with a yield of 87%.

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Abstract

The invention discloses a preparation method of gemfibrozil crystal I, comprising the steps of 1), adding 10 g of gemfibrozil into 20-50 ml of ethanol, and mixing until gemfibrozil dissolves; 2) crystallizing in any one of the manners: I, dropwise adding 20+ / -5 ml of water into the gemfibrozil ethanol solution of step 1), cooling to 10+ / -2 DEG C after dropwise adding, mixing for 1.5-2.5 h, and filtering; II, dropwise adding the gemfibrozil ethanol solution of step 1) to a mixed solvent composed of 12-15 ml of water and 6 ml of ethanol, cooling to 10-20 DEG C after dropwise adding, mixing for 1-2 h, and filtering; 3) drying filter cake, obtained by filtering in step 2), in vacuum at 40+ / -5 DEG C for 7-8 h to obtain gemfibrozil crystal I. The gemfibrozil crystal I prepared via the preparation method has high yield and enables environmental protection burden to be significantly relieved for enterprises.

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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Application Information

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IPC IPC(8): C07C59/68C07C51/43
CPCC07B2200/13C07C51/43C07C59/68
Inventor 许重阳王晖
Owner 浙江精进药业有限公司
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