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Clean preparation method of guanidinoacetic acid

A technology of guanidinoacetic acid and glycine, which is applied in the field of clean preparation of guanidinoacetic acid, can solve the problems of low product purity, difficulty in purification, long synthesis route, increased workload of solvent recovery, etc., and achieve the effect of reducing consumption

Inactive Publication Date: 2013-07-10
北京君德同创生物技术股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In each of the above methods, there are disadvantages such as long synthetic route, low product purity, difficult to purify, and the use of solvents that are prone to pollution, and increase the workload of solvent recovery.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Embodiment 1, prepare guanidinoacetic acid

[0020] In a dry and clean 500mL four-neck flask equipped with a reflux condenser, dropping funnel and thermometer, add 150mL of the recovered mother liquor containing cyanamide and guanidinoacetic acid (wherein glycine and cyanamide are reacted for the first time to prepare guanidine For acetic acid, use water as solvent; the mother liquor obtained in this step reaction is used as the solvent for the next reaction), then add 51.02g glycine, stir and heat, add 28g cyanamide dropwise (in this reaction system, glycine and cyanamide The molar ratio is 1.02:1.00), and the temperature is controlled at 98°C. At this time, liquid ammonia is passed through the reactor to control the pH value at 8.5 and react for 6 hours, then stop the reflux, open the concentration and exhaust steam collection port, and stop after 1 hour. React, start cooling, and when the temperature reaches 20°C, start centrifugation, wash the centrifuged material w...

Embodiment 2

[0023] Embodiment 2, prepare guanidinoacetic acid

[0024] In a dry and clean 500mL four-neck flask equipped with a reflux condenser, dropping funnel and thermometer, add 150mL of the recovered mother liquor containing cyanamide and guanidinoacetic acid (wherein glycine and cyanamide are reacted for the first time to prepare guanidine For acetic acid, use water as the solvent; the mother liquor obtained in this step is the solvent for the next reaction), then add 52.52g of glycine, stir and heat, and drop 28g of cyanamide (in this reaction system, glycine and cyanamide The molar ratio is 1.05:1.00), and the temperature is controlled at 95°C. At this time, liquid ammonia is passed through the reactor to control the pH value at 8.5 and react for 6 hours, then stop the reflux, open the concentration and exhaust steam collection port, and stop after one hour React, start cooling, and when the temperature reaches below 25°C, start centrifugation, and wash the centrifuged material w...

Embodiment 3

[0027] Embodiment 3, prepare guanidinoacetic acid

[0028] In a dry and clean 500mL four-neck flask equipped with a reflux condenser, dropping funnel and thermometer, add 150mL of the recovered mother liquor containing cyanamide and guanidinoacetic acid (wherein glycine and cyanamide are reacted for the first time to prepare guanidine In the case of acetic acid, use water as the solvent; the mother liquor obtained in this step reaction is used as the solvent for the next reaction), then add 54.02g glycine, stir and heat, and drop 28g cyanamide (in this reaction system, glycine and cyanamide The molar ratio is 1.05:1.00), and the temperature is controlled at 96°C. At this time, liquid ammonia is passed through the reactor to control the pH value at 8.5 and react for 6 hours, then stop the reflux, open the concentration and exhaust steam collection port, and stop after 1 hour React, start cooling, and when the temperature reaches below 25°C, start centrifugation, wash the centri...

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Abstract

The invention discloses a preparation method of guanidinoacetic acid. The method comprises the following steps: performing reaction on glycine and hydrogen cyanamide under the alkaline condition; and performing centrifugal separation on the reaction system after reacting, thereby obtaining a solid phase and a liquid phase, wherein the solid phase is guanidinoacetic acid while the liquid phase is a solvent. The method has the advantages that (1) the clean solvent is adopted, and solvent resulting in environmental pollution is not utilized; (2) the raw material matched with hydrogen cyanamide is excessive properly, so that hydrogen cyanamide can react fully and completely; (3) based on the characteristics of hydrogen cyanamide, the reaction solution is concentrated, so that possible trace waste gases can be removed; and (4) a centrifugation mother solution is recycled totally, so that the zero discharge is achieved. Therefore, the environmental protection requirement is satisfied while ammonia and guanidine acetic acid in the mother solution are recycled. As a result, the yield is improved; and the consumption is lowered.

Description

technical field [0001] The invention relates to a clean preparation method of guanidinoacetic acid, which belongs to the technical field of organic synthesis. Background technique [0002] Guanidinoacetic acid is a white crystalline powder. Currently, there are five main preparation methods: 1. S-ethylthiourea hydrobromide is generated by reacting thiourea with ethyl bromide, and then reacted with glycine to prepare guanidinoacetic acid. Mix thiourea, ethyl bromide and absolute ethanol and warm in a water bath for 3 hours to dissolve all thiourea. Then distill off ethanol and excess bromoethane under reduced pressure, crystallize the residue, and dry to obtain S-ethylthiourea hydrobromide. Then add the sodium hydroxide solution into the obtained S-ethylthiourea hydrobromide, cool down, and quickly add the hot solution made of glycine and water. After crystallization, diethyl ether was added and left overnight, the mixture was cooled in an ice bath for 2 h, and the diethyl ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C277/08C07C279/14
Inventor 杨立彬张德福李轶明
Owner 北京君德同创生物技术股份有限公司
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