Refining method of metformin hydrochloride

A technology of metformin hydrochloride and refined products, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of product purity and impurity content that are difficult to meet requirements, purity cannot meet requirements, and environmental pollution is large. Simple and easy to control, less pollution, easy to deal with

Inactive Publication Date: 2019-09-03
WUHAN WUYAO PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0009] The production of metformin hydrochloride in the prior art has defects such as that the purity cannot meet the requirements, the cost is high, and the environmental pollution is large. The most important thing is that the product purity and impurity content after the addition reaction of dicyandiamide and dimethylamine hydrochloride are difficult to meet the requirements. A kind of refining method of metformin hydrochloride is imminent

Method used

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  • Refining method of metformin hydrochloride

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preparation example Construction

[0042] The embodiment of the present invention relates to a method for preparing metformin hydrochloride, through refining the crude metformin hydrochloride, the key impurity dicyandiamide can be completely removed. Specifically, at least the following steps are included:

[0043] (1) adopt solvent method to prepare metformin hydrochloride crude product;

[0044] (2) Add absolute ethanol I to the crude metformin hydrochloride, raise the temperature until reflux occurs, the reflux temperature is 60-78°C, add water dropwise under the reflux state, that is, the system temperature in the process of adding water is not lower than the reflux temperature, and the system dissolves After clearing, add absolute ethanol II dropwise, and the state of dissolving is clear and translucent without crystals visible to the naked eye, and maintains a reflux state during the dissolving and adding process, that is, the system temperature is not lower than the reflux temperature. Suction filtratio...

Embodiment 1

[0071] (1) the preparation of metformin hydrochloride crude product:

[0072] Add 672g of dicyandiamide, 825g of dimethylamine hydrochloride, and 2515g of cyclohexanol into a 1L three-necked flask, and place it in an oil bath environment. When the temperature rises to 86°C, the solids of the system begin to dissolve, and when the temperature continues to rise to 114°C, the system completely dissolves. Clear, slightly green and transparent, when the temperature rises to 140°C ~ 145°C, the color turns brown, and the reaction is kept at 140°C ~ 145°C for 4 hours. It is observed that crystals precipitate out of the system when the reaction is carried out for about 1 hour, and the addition reaction product Generate gradually. When the heat preservation is over, lower the temperature to 100°C, hold at 100°C for 3 hours, and then filter with suction. The filter cake is soaked twice in absolute ethanol with 2 times the weight of dicyandiamide, and then put into a blast drying oven, an...

Embodiment 2

[0081] Compared with Example 1, the only difference is that the amount of purified water added is 816g.

[0082] The parameters of the metformin hydrochloride refined product finished product that obtains are as shown in table 2.

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Abstract

The invention relates to the technical field of chemical pharmacy, and in particular relates to a preparation method of metformin hydrochloride, the method comprises the following steps: preparing crude metformin hydrochloride by adopting a solvent method; adding absolute ethyl alcohol I into the crude metformin hydrochloride, heating to reflux, dripping water under reflux, dripping absolute ethylalcohol II after the system is dissolved, cooling after the dripping is finished to obtain metformin hydrochloride crystals, and obtaining a metformin hydrochloride refined product through suction filtration, washing and drying. The metformin hydrochloride obtained by the preparation method is a white powdery solid, the purity is more than or equal to 99.99%, the key impurity dicyandiamide can becompletely removed, the quality requirement of the refined metformin hydrochloride can be met, the comprehensive yield is high, the mother liquor treatment is simple, and no pollution is caused to the environment.

Description

technical field [0001] The invention relates to the technical field of chemical pharmacy, in particular to a preparation method of metformin hydrochloride. Background technique [0002] Metformin HCL (Metformin HCL), the molecular formula is C 4 h 12 ClN 5 , whose structure is as follows: [0003] [0004] Metformin hydrochloride is a hypoglycemic drug for treating obesity, unsatisfactory diet control alone and ineffective physical exercise for type II diabetic patients. The drug can not only lower blood sugar, but also reduce weight, and has the effect of reducing hyperinsulinemia. At the same time, it has also been proven to have a clear protective cardiovascular effect, and can be used as the basic drug for the whole course of treatment of patients with type II diabetes. In addition, as a first-line drug for the treatment of type II diabetes, it can form a compound preparation with other oral hypoglycemic drugs, and has a good clinical effect. Therefore, the drug...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C277/08C07C279/26
CPCC07C277/08C07C279/26
Inventor 赵涛涛熊恒磊张伟王成张琦谢国范吴鸣
Owner WUHAN WUYAO PHARMA
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