Refining method of glimepiride bulk drug

A refining method and raw material medicine technology, applied in organic chemistry and other fields, can solve problems such as low purification efficiency and increased content of impurity III, and achieve the effects of improving purification efficiency, mild process conditions, and reducing production costs

Inactive Publication Date: 2020-12-04
CHONGQING CONQUER PHARML
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

During the treatment process, glimepiride is hydrolyzed under alkaline conditions to generate impurity III, resulting in an increase in the content of impurity III
This method has only been filtered twice, and the purification efficiency is not high

Method used

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  • Refining method of glimepiride bulk drug
  • Refining method of glimepiride bulk drug
  • Refining method of glimepiride bulk drug

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] A method for refining a glimepiride bulk drug, comprising the following steps:

[0042] Stir 10 g of crude glimepiride into 600 g of purified water, raise the temperature to 65°C, stir and dissolve until the solution is clear, and filter while hot. Cool the filtrate to 30°C, adjust the pH to 2 with 2mol / L hydrochloric acid to obtain a slurry, keep stirring for 1 hour, centrifuge, filter to obtain a filter cake, rinse with purified water until neutral, and control the water content of the filter cake to 25% .

[0043] Add the filter cake into a mixed solvent of 11 g of dichloromethane and 89 g of acetone, stir and heat up to reflux, filter while hot after 1 hour, rinse the filter cake with acetone, and drain it. Dried at 60°C to obtain 9.50 g of Glimepiride Fine Pharmaceutical.

[0044] The purity of glimepiride refined pharmaceuticals measured by high performance liquid chromatography is 99.423%, and the content of impurity III is 0.237%, such as figure 2 .

Embodiment 2

[0046] Stir 10g of crude glimepiride into 800g of purified water, raise the temperature to 60°C, stir and dissolve until the solution is clear, filter while it is hot, cool the filtrate to 20°C, then adjust the pH to 5 with 3mol / L hydrochloric acid to obtain a slurry, keep it warm After stirring for 1 hour, centrifuge and filter to obtain a filter cake, rinse with purified water until neutral, and control the water content of the filter cake to 40%. Add the filter cake to a mixed solvent of 10 g of dichloromethane and 70 g of acetone, stir and heat up to reflux, filter while hot after 1 hour, rinse the filter cake with acetone, and drain it. Dry at 65°C to obtain 9.43 g of glimepiride.

[0047] The purity of glimepiride refined medicine measured by high performance liquid chromatography is 99.537%, and the content of impurity III is 0.280%, such as image 3 .

Embodiment 3

[0049] Stir 20g of crude glimepiride into 1400g of purified water, raise the temperature to 70°C, stir and dissolve until the solution is clear, filter while it is hot, cool the filtrate to 25°C, adjust the pH to 3 with 1mol / L hydrochloric acid to obtain a slurry, keep stirring After 1 hour, centrifuge and filter to obtain a filter cake, rinse with purified water until neutral, and control the water content of the filter cake to 30%.

[0050]Add the filter cake into a mixed solvent of 20 g of dichloromethane and 160 g of acetone, stir and heat up to reflux, and filter while hot after reflux for 2 hours. The filter cake is rinsed with acetone and drained. Dry at 60°C to obtain 18.92 g of glimepiride.

[0051] The purity of glimepiride refined pharmaceuticals measured by high performance liquid chromatography is 99.621%, and the content of impurity III is 0.211%, such as Figure 4 .

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Abstract

The invention provides a refining method of a glimepiride bulk drug, which comprises the following steps: (1) dissolving a glimepiride crude product in purified water, and filtering to obtain a filtrate, (2) acidifying the filtrate to generate slurry, filtering to obtain filter cake, and leaching the filter cake with purified water until the filter cake is neutral, and (3) adding the filter cake into a solvent, stirring, heating to reflux, keeping the reflux condition for 1-2 hours, filtering while the filter cake is hot, leaching with acetone, draining and drying to obtain the glimepiride fine medicine meeting the medicinal standard. The refining method of the glimepiride bulk drug provided by the invention is high in purification efficiency, simple and convenient in operation steps, mildin process conditions, low in production cost and more suitable for large-scale production.

Description

technical field [0001] The invention relates to the technical field of pharmacy, in particular to a method for refining glimepiride raw materials. Background technique [0002] Glimepiride was first launched in Sweden in 1995 by the German company Hoechst Marion Roussel under the trade name Glimepiride is the third-generation sulfonylurea long-acting antidiabetic drug, which can inhibit hepatic glucose synthesis, promote the uptake of peripheral glucose by muscle tissue and promote insulin secretion, and is suitable for simple diet control, exercise therapy and weight loss Patients with type 2 diabetes whose blood sugar is not adequately controlled. [0003] At present, most manufacturers prepare glimepiride according to US4379785: pyrrolidone (5) first reacts with phenylethyl isocyanate (6) to obtain 3-ethyl-4-methyl-2-oxo-N- (2-phenylethyl)-3-pyrroline-1-carboxamide (4), then sulfonated with chlorosulfonic acid to obtain sulfonyl chloride (3), then reacted with ammonia ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D207/38
CPCC07D207/38
Inventor 陈用芳宋世戈胡延贵
Owner CHONGQING CONQUER PHARML
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