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The preparation method of creatine hydrochloride

A technology of creatine hydrochloride and anhydrous creatine, which is applied in the field of preparation of creatine hydrochloride, can solve the problems of post-processing, unfavorable environment, and high production cost, and achieve low cost, short cycle and high yield Effect

Active Publication Date: 2015-11-18
太仓市新毛涤纶化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The use of thionyl chloride and acetyl chloride will also produce other side reaction products mixed into the target product, which will bring many disadvantages to post-processing and the environment, and the preparation cost will also increase

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Add 535kg of absolute ethanol to the reaction kettle, start stirring, add 300kg of anhydrous creatine at one time, cool the material in the kettle to 0°C, slowly add 236kg of absolute ethanol solution containing HCl36%, control the reaction temperature at 0- Between 5°C, after adding the hydrogen chloride ethanol solution, continue to stir for 30 minutes, the reaction time is 2.5 hours, cool the reaction material to 0°C, precipitate crystals, and centrifuge the reaction solution to separate solid and liquid. The mother liquor was reserved for recycling, and the crystals were placed in a vacuum desiccator and dried under reduced pressure at 40°C to obtain 374kg of the target product creatinine hydrochloride with a yield of 97.5%.

[0019] Detected by HPLC: the purity is 99.8%, and the creatinine hydrochloride is less than 100ppm.

Embodiment 2

[0021] Add 700kg of absolute ethanol to the reaction kettle, start stirring, add 400kg of anhydrous creatine at one time, cool the material in the kettle to 0°C, slowly add 306kg of absolute ethanol solution containing HCl37%, control the reaction temperature at 0- Between 5°C, after adding the hydrogen chloride ethanol solution, continue to stir for 30 minutes, the reaction time is 3.5 hours, cool the reaction material to 0°C, and precipitate crystals, centrifuge the solid-liquid separation of the reaction solution, and save the mother liquor for the next preparation For use, the crystals were placed in a vacuum desiccator and dried under reduced pressure at 45° C. to obtain 500 kg of the target product, creatinine hydrochloride, with a yield of 97.8%.

[0022] Detected by HPLC: the purity is 99.9%, creatine hydrochloride is less than 100PPm.

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PUM

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Abstract

The invention relates to a preparation method of creatine hydrochloride. The preparation method sequentially comprises the following steps of: (1) adding anhydrous creatine into absolute ethyl alcohol while stirring; (2) controlling the temperature to be below 10 DEG C, adding an absolute ethyl alcohol solution containing hydrogen chloride into a feed liquid obtained in the step (1), and stirring to generate creatine hydrochloride, wherein the molar rate of the anhydrous creatine to the hydrogen chloride is 1:(1.01-1.02); (3) separating and drying the generated creatine hydrochloride to obtain the creatine hydrochloride. The preparation method is simple in process, short in period and free of use of acyl chloride chemicals, and therefore no decomposition products of the acyl chloride chemicals exists. The steps of heating, distillation and concentration and washing with the an organic solvent are not needed in the reaction, and therefore the preparation method is environmentally-friendly; the target product, namely the creatine hydrochloride, is high in purity, high in yield and low in cost.

Description

technical field [0001] The invention relates to a preparation method of guanidine derivatives, in particular to a preparation method of creatine hydrochloride. Background technique [0002] Creatine is a good nutritional product for human muscles. It can be used in functional drinks, food additives, health products and medicines. Its efficacy is recognized and accepted by people. While the demand is increasing, the requirements for product quality and purity are also increasing. higher. However, creatine has very little solubility in water, which limits its application. Therefore, it is often made into organic acid salts or inorganic acid salts to increase its solubility in water and expand its application range. Creatine hydrochloride is highly soluble in water, so it is valued by people. [0003] The current preparation method of creatine hydrochloride, one is to react creatine monohydrate and 30% hydrochloric acid at a temperature of 25°C to 40°C as disclosed in CN10140...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C279/14C07C277/08
Inventor 张建忠
Owner 太仓市新毛涤纶化工有限公司