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Preparation method of 2-guanidino phenylpropionic acid

A technology of guanidinophenylpropionic acid and phenylalanine, which is applied in the field of preparation of 2-guanidinophenylpropionic acid, can solve problems such as no synthetic method, and achieve the effect of increasing yield

Inactive Publication Date: 2018-02-23
宁夏天成生化科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is currently no synthetic method for this compound

Method used

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  • Preparation method of 2-guanidino phenylpropionic acid
  • Preparation method of 2-guanidino phenylpropionic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Put 100Kg of phenylalanine and 200Kg of purified water into the reactor and mix them well, then adjust the pH value of the system to 8 with liquid caustic soda, then slowly raise the temperature of the reactor to 60°C and start adding 84.83Kg of 30% cyanamide dropwise For aqueous solution, control the dropping rate to 100L / h. After the addition of cyanamide is completed, keep the temperature at T=80°C for 2 hours, lower the temperature of the system to below 20°C and adjust the pH of the system to 8 with hydrochloric acid, and then start centrifugation. The solid was rinsed with ethanol, and the dried target product was 106Kg, the total yield was 84.5%, and the detection purity was 99.3%.

Embodiment 2

[0020] Put 100Kg of phenylalanine and 200Kg of purified water into the reactor and mix them well, then adjust the pH value of the system to 9 with liquid caustic soda, then slowly raise the temperature of the reactor to 70°C and start adding 84.83Kg of 30% cyanamide dropwise For aqueous solution, control the dropping rate to 120L / h. After the addition of cyanamide is completed, keep the temperature at T=80°C for 2 hours, lower the temperature of the system to below 20°C and adjust the pH of the system to 7 with hydrochloric acid, and then start centrifugation. The solid was rinsed with ethanol, and 110Kg of the target product was dried, with a total yield of 87.7% and a detection purity of 99.2%.

Embodiment 3

[0022] Put 100Kg of phenylalanine and 200Kg of mother liquor into the reaction kettle and mix them thoroughly, then adjust the pH value of the system to 9 with liquid caustic soda, then slowly raise the temperature of the reaction kettle to 70°C and start adding 101.80Kg of 30% cyanamide aqueous solution dropwise , control the dropping rate to 120L / h, after the addition of cyanamide, keep the temperature at T=80°C for 2h, lower the temperature of the system to below 20°C, adjust the pH of the system to 7 with hydrochloric acid, then start centrifugation, after centrifugation The solid was rinsed with ethanol, and 115Kg of the target product was dried, with a total yield of 91.7% and a detection purity of 99.5%.

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Abstract

The invention relates to a synthetic method of novel chemicals, in particular to a preparation method of 2-guanidino phenylpropionic acid. The preparation method comprises the main steps: step one, stirring and mixing phenylalanine with purified water, thus forming a mixed solution; step two, regulating the PH (Potential of Hydrogen) value of the mixed solution to be 8 to 10 by using liquid caustic soda; step three, starting to dropwise add hydrogen cyanamide while rising the temperature of the mixed solution obtained in the step two to 60 to 80 DEG C; step four, starting to cool to 20 DEG C or less after keeping warm for 2 hours; step five, regulating the PH value of the mixed solution to be 6 to 8 by using hydrochloric acid; step six, centrifuging, drying and packaging. The 2-guanidino phenylpropionic acid is a new compound, a small amount of information shows that the 2-guanidino phenylpropionic acid is a derivative of aromatic amino acid needed by a human body, and the 2-guanidinophenylpropionic acid has a very important function in the fields of medicinal intermediates, food and feed. According to the preparation method disclosed by the invention, the 2-guanidino phenylpropionic acid is produced by adopting the phenylalanine, the liquid caustic soda, the hydrochloric acid and the hydrogen cyanamide as main raw materials, and the preparation method has the advantages thatthe technology is simple, the reaction is mild, the yield is high, the product purity is high, greening and environment protection are realized, and the like.

Description

technical field [0001] The invention relates to a synthesis method of novel chemicals, in particular to a preparation method of 2-guanidinophenylpropionic acid. technical background [0002] 2-Guanidinophenylpropionic acid is a new compound. There is a small amount of information showing that it is a derivative of an essential aromatic amino acid for the human body. , hypoglycemic, antiviral and anticancer effects, and in the field of bodybuilding, it has the effects of increasing muscle and energy reserves. It can be seen that the compound plays an extremely important role in the fields of pharmaceutical intermediates, food and feed. But there is no synthetic method of any kind of this compound at present. Contents of the invention [0003] The invention aims at the vacancy in the existing 2-guanidinophenylpropionic acid preparation technology, and provides a preparation method of 2-guanidinophenylpropionic acid with simple process, low cost, high yield and high product...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C277/08C07C279/14
Inventor 李江
Owner 宁夏天成生化科技有限公司
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