Metformin hydrochloride purification method

A technology of metformin hydrochloride and purification method, which is applied in the field of purification of metformin hydrochloride, and can solve the problems of increased operation difficulty and high purification cost

Active Publication Date: 2009-06-10
JIANGSU DEYUAN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The production route usually adopted by this medicine is to synthesize dimethylamine hydrochloride from dimethylamine and hydrochloric acid, then synthesize the crude metformin hydrochloride from dimethylamine hydrochloride and dicyandiamide, and refine the crude metformin hydrochloride with 95% ethanol, which is easy to clog during press filtration The filter press pipeline needs to be kept warm on the filter press pipeline, and it takes 2 hours to press filter 200Kg of metformin hydrochloride material, which increases the difficulty of operation, and the purification cost is relatively high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] Prepare 235Kg of industrial hydrochloric acid in the high-level tank, add 200Kg of dimethylamine into the reaction tank, start stirring, turn on the ice brine to cool down, close the vacuum, open the vent valve, start adding hydrochloric acid dropwise to PH=3, close and press back to the cooling brine, Turn on the vacuum, turn on the steam to heat and remove the water, until no moisture comes out. Then suck in 260Kg of isoamyl alcohol, turn off the vacuum, open the mouth of the reaction tank and add 150Kg of dicyandiamide, and cover the feeding port tightly. Turn on the steam to heat and reflux for 12 hours, close the steam valve, cool the condensed water to below 50°C, shake off the material, reclaim the mother liquor, wash the material with 40Kg of absolute ethanol, and obtain 280Kg of metformin hydrochloride crude product. Put the obtained metformin hydrochloride crude product and 840Kg of purified water 3 times its weight into a reaction tank, heat it to 65°C and re...

Embodiment 2

[0012] Prepare 235Kg of industrial hydrochloric acid in the high-level tank, add 200Kg of dimethylamine into the reaction tank, start stirring, turn on the ice brine to cool down, close the vacuum, open the vent valve, start adding hydrochloric acid dropwise to PH=3, close and press back to the cooling brine, Turn on the vacuum, turn on the steam to heat and remove the water, until no moisture comes out. Then suck in 260Kg of isoamyl alcohol, turn off the vacuum, open the mouth of the reaction tank and add 150Kg of dicyandiamide, and cover the feeding port tightly. Turn on the steam to heat and reflux for 12 hours, turn off the steam valve, cool the condensed water to below 50°C, shake off the material, reclaim the mother liquor, wash the material with 50Kg of absolute ethanol, and obtain 279Kg of metformin hydrochloride crude product. Put the obtained metformin hydrochloride crude product and 837Kg of purified water 3 times its weight into a reaction tank, heat it to 75°C and...

Embodiment 3

[0014] Prepare 235Kg of industrial hydrochloric acid in the high-level tank, add 200Kg of dimethylamine into the reaction tank, start stirring, turn on the ice brine to cool down, close the vacuum, open the vent valve, start adding hydrochloric acid dropwise to PH=3, close and press back to the cooling brine, Turn on the vacuum, turn on the steam to heat and remove the water, until no moisture comes out. Then suck in 260Kg of isoamyl alcohol, turn off the vacuum, open the mouth of the reaction tank and add 150Kg of dicyandiamide, and cover the feeding port tightly. Turn on the steam to heat and reflux for 12 hours, turn off the steam valve, cool the condensed water to below 50°C, shake off the material, reclaim the mother liquor, wash the material with 45Kg of absolute ethanol, and obtain 285Kg of metformin hydrochloride crude product. Put the obtained metformin hydrochloride crude product and 855Kg of purified water 3 times its weight into a reaction tank, heat it to 70°C and...

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PUM

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Abstract

The invention discloses a method for purifying metformin hydrochloride in the technical field of chemical synthesis. The invention adopts a technical proposal that: a crude product of metformin hydrochloride obtained through synthesis of dimethylammonium chloride and dicyandiamide is put into a purified water of which the weight is three times of that of the crude product of metformin hydrochloride, heated to 65 to 75 DEG C for circumfluence to be dissolved completely, and then is cooled to separate a mother liquid; and thus refined metformin hydrochloride is obtained. The obtained product avoids blocking the filter press pipes easily, and does not need heat preservation in the filter press pipes, filter press of 200kg of metformin hydrochloride takes about 0.5 hour, and the method has easy operation and decreased cost.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, in particular to a method for purifying metformin hydrochloride. Background technique [0002] Metformin Hydrochloride (Metformin Hydrochloride) has strong physiological activity, and it is a hypoglycemic drug with definite curative effect for clinical use. It mainly acts on tissues outside the pancreas, inhibits the intestinal absorption of glucose, increases the utilization of glucose by peripheral tissues, and reduces hepatic gluconeogenesis, thereby achieving the effect of lowering blood sugar. Not only has a unique therapeutic effect on Type 2 diabetes, but pharmacological studies have proved that it can also significantly lower blood pressure and reduce glutathione in the blood and Mg in the liver. 2+ Concentration, has the function of protecting the liver. Therefore, metformin hydrochloride is a chemosynthetic substance with broad-spectrum therapeutic effects. [0003] The production r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C279/26C07C277/06
Inventor 马方兴仝翔
Owner JIANGSU DEYUAN PHARMA
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