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Method for preparing creatine in catalyzed mode

A technology for catalytic preparation of creatine, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of unsatisfactory yield, leakage of highly toxic substances, high production cost, etc., and achieve shortened reaction time, yield The effect of high yield and improved yield

Inactive Publication Date: 2016-01-20
王晓伟
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these traditional preparation methods often involve highly toxic cyanamide or the yield is not ideal, which has great potential safety hazards and high production costs. Especially for large-scale industrial production, the leakage of highly toxic substances is easy to cause Casualties, and at the same time, it does not conform to the spirit of the country's green and environmentally friendly economy

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] (1) Add 1kg of S-methylisothiourea sulfate to the reaction kettle, and add 1.1L of mixed solvent with a water / ethanol volume ratio of 3:1, and slowly heat up to 30°C under stirring;

[0018] (2) Add 80g of 1-allyl-3-butylimidazolium tetrafluoroborate in the above reaction solution, after adding, slowly add 2.5kg of potassium sarcosinate aqueous solution with a mass concentration of 30%, and control the temperature At 25-30°C, drop it within 30 minutes, adjust the pH to 10 with 30% KOH, and react for 3 hours;

[0019] (3) After the reaction is completed, the crude product is obtained by filtration, and the crude product is dissolved with 10% sulfuric acid aqueous solution, and adjusted to neutrality, recrystallized and decolorized with activated carbon, and the yield of creatine is 76%.

Embodiment 2

[0021] (1) Add 1kg of S-methylisothiouronium sulfate to the reaction kettle, and add 1.2L of mixed solvent with a water / ethanol volume ratio of 3:1, and slowly heat up to 30°C under stirring;

[0022] (2) Add 50g of 1-allyl-3-butylimidazolium tetrafluoroborate in the above-mentioned reaction solution, after adding, slowly add 2 kg of potassium sarcosinate aqueous solution with a mass concentration of 30%, and control the temperature at 25-30°C, drop within 20 minutes, adjust the pH to 9 with 30% KOH, and react for 3 hours;

[0023] (3) After the reaction is completed, the crude product is obtained by filtration, and the crude product is dissolved with 10% sulfuric acid aqueous solution, and adjusted to neutrality, recrystallized and decolorized by activated carbon, and the yield of creatine is 74%.

Embodiment 3

[0025] (1) Add 1kg of S-methylisothiourea sulfate to the reaction kettle, and add 1L of mixed solvent with a water / ethanol volume ratio of 3:1, and slowly heat up to 30°C under stirring;

[0026] (2) Add 1-allyl-3-butylimidazolium tetrafluoroborate of 100g in the above-mentioned reaction solution, add, then slowly add mass concentration and be 3kg of potassium sarcosinate aqueous solution of 30%, control temperature at 25-30°C, drop it within 30 minutes, adjust the pH to 10 with 30% KOH, and react for 2 hours;

[0027] (3) After the reaction is completed, the crude product is obtained by filtration, and the crude product is dissolved with 10% sulfuric acid aqueous solution, and adjusted to neutrality, recrystallized and decolorized by activated carbon, and the yield of creatine is 75%.

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Abstract

The invention relates to a method for preparing creatine in a catalyzed mode. According to the method, S-methyl isothiourea sulfate and potassium sarcosinate are adopted as raw materials and are further prepared into creatine, utilization of highly-toxic ammonia cyanide is avoided, and production safety is effectively ensured. Meanwhile, a phase transfer catalyst is added in the reaction process, the reaction is carried out in an alcohol / water system, dissolvability of the materials can be guaranteed, and the sufficient conversion of the materials can be promoted under the action of the catalyst. The method in the technical scheme has the advantages of being environmentally friendly, high in yield and short in reaction time and has a wide industrialization prospect.

Description

technical field [0001] The invention relates to a method for synthesizing creatine, in particular to a method for catalytically preparing creatine, which belongs to the field of organic intermediate synthesis. Background technique [0002] Creatine, also known as creatine monohydrate, has a chemical name of N-methylguanidinoacetic acid. As a sports nutrient, it can significantly improve muscle strength and endurance. Because creatine does not belong to hormone substances, it will not produce drug resistance and physiological side effects, so creatine nutritional preparations are favored by people. [0003] At present, the large-scale production method of creatine mainly contains the following several kinds: (1) the reaction of β-aminoacetic acid and ammonium cyanide prepares creatine, as US2654799A, (2) the reaction preparation of chloroacetic acid, methylamine and cyanamide aqueous solution Creatine, such as CN99122417A, (3) sodium sarcosinate or potassium sarcosinate reac...

Claims

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Application Information

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IPC IPC(8): C07C279/14C07C277/08
Inventor 王晓伟
Owner 王晓伟
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