Preparation method of metformin hydrochloride

A technology of metformin hydrochloride and dicyandiamide, which is applied in the field of medicine and chemical industry, can solve the problems of many side reactions, long reaction cycle and high production cost, and achieve the effects of reducing production cost, suppressing side reactions and increasing yield

Inactive Publication Date: 2016-04-13
SHIJIAZHUANG POLEE PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the reaction time is generally 8h-12h or even longer, the reaction

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] A method for preparing metformin hydrochloride, which is characterized by comprising the following steps:

[0016] Add 100kg of dicyandiamide and 120kg of dimethylamine hydrochloride to a 300L reactor, and then add 300kg of cyclohexanol; start the stirring device, control the speed at 45r / min, adjust the vacuum in the reactor to 0.08MPa, and heat to 140℃ After reacting for 3 hours, a crude product of metformin hydrochloride is obtained; the crude product is recrystallized with ethanol, filtered and dried to obtain metformin hydrochloride.

[0017] After testing, the mass of the obtained metformin hydrochloride was 89.3 kg, the yield was 94.8%, and the purity was 99.5%.

Embodiment 2

[0019] A method for preparing metformin hydrochloride, which is characterized by comprising the following steps:

[0020] Add 100kg of dicyandiamide and 120kg of dimethylamine hydrochloride to a 300L reactor, and then add 300kg of cyclohexanol; start the stirring device, control the speed at 50r / min, adjust the vacuum in the reactor to 0.10MPa, and heat to 135℃ After reacting for 2 hours, a crude product of metformin hydrochloride is obtained; the crude product is recrystallized with ethanol, filtered and dried to obtain metformin hydrochloride.

[0021] After testing, the mass of the obtained metformin hydrochloride was 87.3 kg, the yield was 94.0%, and the purity was 99.3%.

Embodiment 3

[0023] A method for preparing metformin hydrochloride, which is characterized by comprising the following steps:

[0024] Add 100kg of dicyandiamide and 120kg of dimethylamine hydrochloride to a 300L reactor, and then add 300kg of cyclohexanol; start the stirring device, control the speed at 47r / min, adjust the vacuum in the reactor to 0.09MPa, and heat to 145°C After reacting for 2.5 hours, a crude product of metformin hydrochloride is obtained; the crude product is recrystallized with ethanol, filtered and dried to obtain metformin hydrochloride.

[0025] After testing, the mass of the obtained metformin hydrochloride was 88.6 kg, the yield was 94.5%, and the purity was 99.4%.

[0026] The preparation method for preparing metformin hydrochloride of the present invention requires only 2 to 3 hours of reaction time, which greatly shortens the reaction time and reduces the production cost; it can effectively inhibit the generation of side reactions and reduce the content of impurities...

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PUM

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Abstract

The invention discloses a preparation method of metformin hydrochloride. The method is characterized by including the following steps of firstly, adding dicyandiamide and dimethylamine hydrochloride in a reaction still, and adding cyclohexanol, wherein the mole ratio of dicyandiamide to dimethylamine hydrochloride is 1:1.2, and the mole ratio of cyclohexanol to dicyandiamide is 3:1; secondly, starting a stirring device, controlling the rotating speed at 45-50 r/min, regulating the vacuum degree in the reaction still to 0.08-0.09 MPa, heating the mixture to 135-145 DEG C, and preparing crude metformin hydrochloride after the reaction is conducted for 2.5 hours; thirdly, conducting recrystallization on the crude product through ethyl alcohol, and conducting filtering and drying to obtain the metformin hydrochloride. By means of the method, the reaction time is greatly shortened, the production cost is reduced, side reactions can be effectively restrained, the impurity content is reduced, and therefore the yield of the product is greatly improved.

Description

Technical field [0001] The invention belongs to the field of medicine and chemical industry, and specifically relates to a preparation method of metformin hydrochloride. Background technique [0002] Metformin Hydrochloride (Metformin Hydrochloride), a safe and effective blood pressure lowering and blood sugar lowering drug. Especially in the process of preventing diabetes, metformin hydrochloride has been used more and more widely, becoming an irreplaceable oral hypoglycemic agent. The drug can be used in combination with insulin, which can enhance the hypoglycemic effect of insulin, thereby reducing the amount of insulin; the drug can also be used in combination with sulfonylureas oral hypoglycemic drugs, which has a synergistic effect. [0003] At present, the synthetic methods of metformin hydrochloride mainly include melting method and solvent method. The melting method uses solid materials in the early and late stages of the reaction, which requires high equipment performan...

Claims

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Application Information

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IPC IPC(8): C07C279/26C07C277/08
CPCC07C277/08C07C279/26
Inventor 秦晓辉秦建辉杨旭翠
Owner SHIJIAZHUANG POLEE PHARMA CO LTD
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