Metformin hydrochloride synthesis
- Product Name:Metformin hydrochloride
- CAS Number:1115-70-4
- Molecular formula:C4H12ClN5
- Molecular Weight:165.62
124-40-3
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Yield:1115-70-4 96.3%
Reaction Conditions:
with hydrogenchloride;sodium methylate in methanol;water at 5 - 30; for 5 h;Solvent;Temperature;
Steps:
1-4; 1-3 Example 1 A synthetic method of metformin hydrochloride A1
This example provides a method for synthesizing metformin hydrochloride A1. The method is to weigh 16.8 g of dicyandiamide and add it to 50 ml of methanol to dissolve. After stirring, add 9.1 g of dimethylamine. After stirring to dissolve, add 27 g of sodium methoxide. Every ten minutes, increase the temperature by 5°C to the reaction temperature of 30°C, keep it warm and stir for 5h, take a small amount of the reaction solution after 5h, monitor the reaction process by ion chromatography after dilution, the ion peak of dicyandiamide disappears, a new peak appears, and the molecular weight is 130.17 (M+), this peak is the ion peak of metformin, which is the end of the reaction. After the reaction, the methanol is concentrated to dryness. After the remaining materials were cooled to room temperature, 50ml purified water was added, 15ml of hydrochloric acid with a concentration of 38% was added dropwise, the pH was adjusted to 3, after mixing and stirring, 200ml ethyl acetate was added, and after mixing and stirring for 20 minutes, the mixture was allowed to stand and separate, the organic phase Concentrated and recovered, dried with anhydrous sodium sulfate, can be used for the next synthesis; the resulting aqueous phase, Distill under reduced pressure until the remaining solution volume is one-fifth of the original water phase volume, and lower the temperature of the remaining solution to room temperature, add 180ml of ethanol with a concentration of 80%, and after mixing it evenly, stop stirring, put it in the freezer at low temperature Crystallize and filter in an ice-water bath. Dissolve the filter cake again in 20ml purified water, add 100g activated carbon, stir for 10min to decolorize, after filtering, wash the filter cake with 20ml purified water, add 120ml of 80% ethanol again, mix well Afterwards, it was crystallized at low temperature for 7 hours, filtered, and the filter cake was dried to obtain 31.7 g of metformin hydrochloride A1, with a yield of 96.3%.
References:
CN113248409,2021,A Location in patent:Paragraph 0029-0047
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