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Synthetic method of metformin hydrochloride

A technology of metformin hydrochloride and synthesis method, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problem of high reaction temperature, and achieve the advantages of lowering reaction temperature, simplifying purification process, reducing production cost and environmental cost. Effect

Active Publication Date: 2016-09-28
NINGXIA SIKEDA BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

And some other reports mainly focus on utilizing high-boiling solvents, such as isoamyl alcohol, glycerol, n-amyl alcohol, cyclohexanol, etc. to replace xylene for process improvement. In addition to the above-mentioned problems, there is also the overall reaction temperature higher question

Method used

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  • Synthetic method of metformin hydrochloride
  • Synthetic method of metformin hydrochloride
  • Synthetic method of metformin hydrochloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Add 2.3Kg dimethylamine, 4.2Kg dicyandiamide, 5.5Kg of 30% hydrochloric acid aqueous solution successively in 20L reaction kettle with mechanical stirrer, 0.0084Kg mass fraction is 88% formic acid, stir slowly and heat to 130 ℃, Keep warm for 1.5 hours, slowly cool to room temperature;

[0028] (2) Transfer the milky white mixture obtained in step (1) to a 50L glass reactor, add 28Kg 95% ethanol, heat and reflux and stir for 30min and then cool and crystallize. Kg (yield is 93% based on dicyandiamide)

[0029] Depend on figure 1 and figure 2 It can be seen that the product prepared by the present invention is metformin hydrochloride, by image 3 It was found that the purity was higher than 95% as can be seen by high performance liquid chromatography.

Embodiment 2

[0031] (1) Add 2.3Kg dimethylamine, 4.2Kg dicyandiamide, 5.5Kg of 30% hydrochloric acid aqueous solution, 0.0084Kg mass fraction 88% formic acid successively in 20L reaction kettle with mechanical stirrer, stir slowly and heat to 120 ℃, keep warm 1.5 hours, slowly cool to room temperature;

[0032] (2) Transfer the milky white mixture obtained in step (1) to a 50L glass reactor, add 28Kg 95% ethanol, heat and reflux and stir for 30min, then cool and crystallize, after the white solid is centrifuged, vacuum-dry to obtain white metformin hydrochloride 7.45 Kg (yield is 91% based on dicyandiamide)

[0033] Depend on Figure 4 It was found that the purity was higher than 95% as can be seen by high performance liquid chromatography.

Embodiment 3

[0035] (1) Add 2.3Kg dimethylamine, 4.2Kg dicyandiamide, 8.3Kg of 20% hydrochloric acid aqueous solution, 0.0084Kg mass fraction 88% formic acid successively in a 20L reaction kettle with a mechanical stirrer, stir slowly and heat to 130°C, keep warm 1.5 hours, slowly cool to room temperature;

[0036] (2) Transfer the milky white mixture obtained in step (1) to a 50L glass reactor, add 28Kg 95% ethanol, heat and reflux and stir for 30min and then cool and crystallize. After the white solid is centrifuged, it is vacuum dried to obtain white metformin hydrochloride 7.3 Kg (yield is 88% based on dicyandiamide)

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Abstract

The invention discloses a synthetic method of metformin hydrochloride. The method comprises the following steps: (1) in a high pressure enclosed environment, dimethylamine, dicyandiamide, a hydrochloric acid solution, and a catalyst organic acid are added, and a heating reaction is carried out in order to obtain metformin hydrochloride; (2) metformin hydrochloride is obtained by refining with ethyl alcohol. The pressure generated by heating in a high pressure reaction vessel is used, so that dimethylamine in a water system and dicyandiamide are reacted in order to generate metformin hydrochloride, reaction temperature is effectively reduced, and according to dicyandiamide, the reaction yield is higher than 90%. Water is used as a reaction solvent, and compared with traditional technology, the method has the advantages of low raw material cost, low toxicity, simple reaction process, low energy consumption, small waste liquid discharge, easy industrial production, and substantially reduced production cost and environment cost . A trace amount of an organic acid catalyst is used, so that stability of dicyandiamide in a high temperature water system is effectively improved, generation of side reaction of cyanamide is reduced, and the purification process is simplified.

Description

technical field [0001] The invention belongs to the field of organic synthesis, in particular to a method for synthesizing metformin hydrochloride. Background technique [0002] Metformin hydrochloride (trade name: Metformin) has been in the treatment of diabetes for half a century since its launch in 1957. Expand and extend. In the latest version (2013) of the ADA (American Diabetes Association) guidelines for diabetes prevention and control, the sequence and path of specific hypoglycemic drugs used in the strategy of controlling hyperglycemia are clarified: Metformin should be used as initial treatment while life intervention is used, and metformin should be used as first-line therapy. Drugs were used throughout the course of treatment, and intensive insulin combined with metformin and glitazones was used as the final treatment. In my country's 2013 edition of the guidelines for the prevention and treatment of diabetes, it is also clearly stated that the drug of choice f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C279/26C07C277/08
CPCC07C277/08C07C279/26
Inventor 田永富陈红余孙风程王科李平
Owner NINGXIA SIKEDA BIOTECH CO LTD
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