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Green preparation method of phthaloylglycyl-l-glutamine

A technology of phthaloyl glycyl and glutamine, which is applied in the field of medicine, can solve the problems of high energy consumption, high requirements for equipment and personnel, harm to the environment and operators, etc., and achieves low cost, green cost and environmental protection. , the effect of reducing investment

Active Publication Date: 2016-01-13
陕西西岳制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The isopropyl chloroformate used in this method is a highly toxic substance, which is extremely harmful to the environment and operators, so the requirements for equipment and personnel are very high in industrial production.
And vacuum distillation needs to consume a lot of energy, discharge toxic and harmful waste gas and waste liquid

Method used

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  • Green preparation method of phthaloylglycyl-l-glutamine
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  • Green preparation method of phthaloylglycyl-l-glutamine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Add 16g of caustic soda and 40g of soda ash to 500mL of water, and add 50g of L-glutamine, stir to dissolve, and cool the resulting reaction solution to -7°C to form a solution. Phthaloylglycyl chloride was rapidly added dropwise at a rate of 2.5 g / s, during which the temperature of the reaction solution was controlled between 9 and 10°C. After the dropwise addition, the reaction was stirred for 60 minutes. Then slowly add 12 mol / L hydrochloric acid solution to the solution, adjust the pH to 4, stir for 9 minutes, and a large amount of white solids are precipitated. Continue to dropwise add 0.2 mol / L hydrochloric acid solution to the reaction solution, adjust the pH to 1.5, and completely precipitate the product, and stir for 5 minutes. The solid was filtered and dried to obtain 111.9 g of the product phthalylglycyl-L-glutamine, with a yield of 98.2%. According to high performance liquid chromatography (HPLC), its phthalylglycyl-L- The purity of L-glutamine is 99.1%. ...

Embodiment 2

[0035] Add 16g of caustic soda and 40g of soda ash to 500mL of water, and add 50g of L-glutamine, stir to dissolve, and cool the resulting reaction solution to -8°C to form a solution. Rapidly phthaloylglycyl chloride at a rate of 2.8g / s, during which the temperature of the reaction solution is controlled between 9 and 10°C. After the dropwise addition, the reaction was stirred for 60 minutes. Then slowly add 12 mol / L hydrochloric acid solution to the solution, adjust the pH to 3, stir for 9 minutes, and a large amount of white solids are precipitated. Continue to dropwise add 0.2 mol / L hydrochloric acid solution to the reaction solution, adjust the pH to 1.5, and completely precipitate the product, and stir for 5 minutes. The solid was filtered and dried to obtain 112.3 g of the product phthaloylglycyl-L-glutamine, with a yield of 98.5% and an HPLC purity of 99.2%.

Embodiment 3

[0037] Add 18g of caustic soda and 40g of soda ash to 500mL of water, add 50g of L-glutamine, stir to dissolve, and cool the resulting reaction solution to -7°C. Rapidly phthaloylglycyl chloride at a rate of 2.8g / s, during which the temperature of the reaction solution is controlled between 9 and 10°C. After the dropwise addition, the reaction was stirred for 60 minutes. Then, 6N sulfuric acid solution was slowly added to the solution to adjust the pH to 3, and stirred for 9 minutes, and a large amount of white solid was precipitated. Continue to add 0.2 mol / L hydrochloric acid solution dropwise to the reaction solution, adjust the pH to 2, and completely precipitate the product, and stir for 5 minutes. The solid was filtered and dried to obtain 111.9 g of the product phthaloylglycyl-L-glutamine, with a yield of 98.2% and an HPLC purity of 99.3%.

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Abstract

The invention discloses a green preparation method of phthalylglycyl-L-glutamine, which comprises the following steps: reacting raw materials phthalylglycyl chlorine and L-glutamine in an inorganic alkali water solution, acidifying twice, crystallizing, filtering and drying to obtain the product. The preparation method has the advantages of accessible raw materials, high product yield and high product purity, is simple to operate, avoids using toxic and harmful organic solvents, effectively lowers the emissions of waste water, waste liquid and waste gas in industrial production, and reduces the environmental pollution. The high-purity phthalylglycyl-L-glutamine prepared by the method provides a reliable raw material for further synthesizing ultrahigh-purity glycyl glutamine, thereby effectively lowering the clinical side effect of the glycyl glutamine preparation.

Description

technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a green preparation method of phthaloylglycyl-L-glutamine. Background technique [0002] Glycyl glutamine is also known as N-glycyl-L-glutamine (formula 1), molecular formula C 7 h 13 N 3 o 4 , molecular weight 202.1. [0003] [0004] Glycylglutamine is an important component of parenteral nutrition drugs, which can effectively enhance the patient's cellular immune function and reduce the risk of infection in patients. Therefore, it is widely used in the treatment of intestinal insufficiency, severe infection, burns, immunodeficiency syndrome, etc. Glycylglutamine can be decomposed into glutamine and alanine in the human body. Therefore, Professor Peter proposed a concept of dipeptide, that is, alanine and glutamine are used to form glutamic dipeptide, and the prepared preparation is used as glutamine A donor of aminoamide, which meets the patient's needs t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07K5/078C07K1/02
Inventor 孔凯明王维郑贝贝
Owner 陕西西岳制药有限公司
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