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Preparation method of alanyl glutamine

A technology of alanyl glutamine and glutamine, which is applied in the field of preparation of alanyl glutamine, can solve the problems of low yield of finished products, cumbersome steps, time-consuming and other problems, and achieve convenient and high yield , instruments, and simple conditions

Inactive Publication Date: 2021-03-30
南京肽谷生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method steps are cumbersome, time-consuming and consumable in the preparation process, and the yield of finished products is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] A preparation method of alanyl glutamine comprises the following steps in sequence:

[0021] S1: Preparation of chloropropionyl-glutamine: Add 100 mL of ddH to a stirred tank under alkaline conditions 2 0, 100mL toluene, the alkali is one of sodium hydroxide, potassium hydroxide, calcium hydroxide, and adjust the pH to 10.3, stir for 5min, then add 30ml of glutamine, mix well and lower the temperature to 0-4 ℃, keep 1-1.5h, then raise the temperature to 15-20℃, keep 2-4h, add strong acid to the water layer to adjust the pH to 1.5, strong acid includes concentrated sulfuric acid, concentrated hydrochloric acid, lower the temperature to 0-4℃ and let it stand for 24-36h , filtered out the crystals to obtain white crystals of chloropropionyl-glutamine, the filtrate was evaporated at high temperature to remove the solvent, and then cooled and crystallized to obtain white crystals of chloropropionyl-glutamine, white crystals of chloropropionyl-glutamine Carry out drying trea...

Embodiment 2

[0025] A preparation method of alanyl glutamine comprises the following steps in sequence:

[0026] S1: Preparation of chloropropionyl-glutamine: add 100-300mLddH to a stirred tank under alkaline conditions 2 0, 100-300mL toluene, alkali is a kind of in sodium hydroxide, potassium hydroxide, calcium hydroxide, and adjust pH to be 10.5, carry out stirring 5min, then add 70g glutamine again, after mixing well, reduce temperature to 0 -4°C, keep it for 1-1.5h, then raise the temperature to 15-20°C, keep it for 2-4h, add strong acid to the water layer to adjust the pH to 1.5, strong acid includes concentrated sulfuric acid, concentrated hydrochloric acid, lower the temperature to 0-4°C and let stand for 24 -36h, the crystals were filtered out to obtain white crystals of chloropropionyl-glutamine. Aminoamide is dried and then preserved for subsequent use;

[0027] S2: Preparation of crude product of alanyl glutamine: Take 150 g of chloropropionyl-glutamine obtained in the above s...

Embodiment 3

[0030] A preparation method of alanyl glutamine comprises the following steps in sequence:

[0031] S1: Preparation of chloropropionyl-glutamine: Add 300 mL of ddH to a stirred tank under alkaline conditions 20, 300mL toluene, the alkali is a kind of in sodium hydroxide, potassium hydroxide, calcium hydroxide, and adjust pH to be 10.8, carry out stirring 5min, then add 30-100g glutamine, after mixing evenly, reduce temperature to 0 -4°C, keep it for 1-1.5h, then raise the temperature to 15-20°C, keep it for 2-4h, add strong acid to the water layer to adjust the pH to 1.5, strong acid includes concentrated sulfuric acid, concentrated hydrochloric acid, lower the temperature to 0-4°C and let stand for 24 -36h, the crystals were filtered out to obtain white crystals of chloropropionyl-glutamine. Aminoamide is dried and then preserved for subsequent use;

[0032] S2: Preparation of crude product of alanyl glutamine: take 200 g of chloropropionyl-glutamine obtained in the above s...

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PUM

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Abstract

The invention discloses a preparation method of alanyl glutamine, which comprises the following steps: S1: preparation of chloroalanyl glutamine: adding 100-300 mL of ddH2O and 100-300 mL of toluene into a stirring tank under an alkali condition, stirring for 5 minutes, adding 30-100 g of glutamine, uniformly mixing the components, cooling the mixture to 0-4 DEG C, keeping the status for 1-1.5 hours, heating the mixture to 15-20 DEG C, keeping the status for 2-4 hours, and adding strong acid into a water layer to adjust pH to 1.5, then reducing the temperature to 0-4 DEG C, carrying out standing treatment for 24-36 hours, and filtering out crystals to obtain white crystal chloropropionyl glutamine; s2, preparation of an alanyl glutamine crude product; s3, preparation of the alanyl glutamine. According to the preparation method of the alanyl glutamine, the target product can be obtained by adopting three steps, the time is saved, the raw materials are convenient to obtain, instruments and conditions used in the preparation process are simple and convenient to obtain, and the yield of the prepared finished product is high.

Description

technical field [0001] The invention belongs to the technical field of medicine preparation, and in particular relates to a preparation method of alanyl glutamine. Background technique [0002] The molecular formula of alanylglutamine is C8H15N3O4, which is a white or off-white loose lump. As a parenteral nutrition drug, it can be used to improve the patient's cellular immune function and effectively reduce the risk of infection in critically ill patients, especially for severe infections and malignant tumors. The treatment and recovery of critically injured patients plays an important role in reducing the total length of hospital stay for patients. CG dipeptide is widely used in foreign countries. Since its introduction in my country, its market demand is increasing and the market prospect is broad. [0003] The synthesis method reported in the literature has the DCC coupling method, Boc-alanine and N-hydroxysuccinimide are condensed under DCC conditions, and the dicyclohe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07K5/062C07K1/30C07K1/14
CPCC07K5/06026C07K2299/00
Inventor 王滋善张厚之
Owner 南京肽谷生物科技有限公司
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