Methanol recycling method in production process of N(2)-L-alanyl-L-glutamine

A technology for phthaloyl alanyl glutamine and glutamine, which is applied in the field of synthesis and preparation of medicines, can solve the problems of ineffective recovery and treatment of waste methanol, restrict product production, affect product yield and the like, and achieve elimination of Environmental regulations risk, the effect of reducing product production costs, and reducing disposal costs

Inactive Publication Date: 2017-09-15
山东辰龙药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the conventional production process of this drug on the market is chemical synthesis, that is, using phthalylalanyl glutamine and hydrazine hydrate as raw materials to undergo a chemical reaction to synthesize the product, and the product is purified and refined by methanol crystallization, because the synthesis process There are more raw materials in the medium, resulting in the synthesis of N(2)-L-alanyl-L-glutamine aqueous solution containing impurities, these impurities when N(2)-L-alanyl-L-glutamine crystallization In the used methanol, these impurities are distilled into the recovered methanol along with the methanol vapor during the methanol distillation recovery operation. There is no effective way to separate them. The recovered methanol containing impurities is in the N(2)-L-alanyl-L- During the use of glutamine, it seriously affects the product yield of N(2)-L-alanyl-L-glutamine and affects the use of recovered methanol. Under the situation of increasingly severe environmental supervision, N(2) -The waste methanol produced in the production process of L-alanyl-L-glutamine cannot be effectively recycled and treated, which greatly restricts the production of the product

Method used

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  • Methanol recycling method in production process of N(2)-L-alanyl-L-glutamine

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Embodiment 1

[0025] The methanol recycling method in the N(2)-L-alanyl-L-glutamine production process of the present invention comprises the following steps:

[0026] (1) Collection of N(2)-L-alanyl-L-glutamine aqueous solution: put phthalylalanyl glutamine, hydrazine hydrate, and methanol into the reaction kettle for chemical reaction, after the reaction is completed The product is centrifuged in a centrifuge, the solid material produced is collected, the collected solid material is dissolved in water, stirred evenly and centrifuged, and the N(2)-L-alanyl-L-glutamine aqueous solution is collected;

[0027] (2) Distillation under reduced pressure: put the collected N(2)-L-alanyl-L-glutamine aqueous solution into a glass-lined reactor, close all valves of the glass-lined reactor, turn on the vacuum, and carry out vacuum distillation. During the vacuum distillation, keep the temperature in the glass-lined reactor at 60°C, the vacuum degree -0.06Mpa, and the vacuum distillation time for 2.5h;...

Embodiment 2

[0032] The methanol recycling method in the N(2)-L-alanyl-L-glutamine production process of the present invention comprises the following steps:

[0033] (1) Collection of N(2)-L-alanyl-L-glutamine aqueous solution: put phthalylalanyl glutamine, hydrazine hydrate, and methanol into the reaction kettle for chemical reaction, after the reaction is completed The product is centrifuged in a centrifuge, the solid material produced is collected, the collected solid material is dissolved in water, stirred evenly and centrifuged, and the N(2)-L-alanyl-L-glutamine aqueous solution is collected;

[0034] (2) Distillation under reduced pressure: put the collected N(2)-L-alanyl-L-glutamine aqueous solution into a glass-lined reactor, close all valves of the glass-lined reactor, turn on the vacuum, and carry out vacuum distillation. During vacuum distillation, keep the temperature in the glass-lined reactor at 60°C, the vacuum degree -0.1Mpa, and the vacuum distillation time is 2h;

[003...

Embodiment 3

[0039] The methanol recycling method in the N(2)-L-alanyl-L-glutamine production process of the present invention comprises the following steps:

[0040] (1) Collection of N(2)-L-alanyl-L-glutamine aqueous solution: put phthalylalanyl glutamine, hydrazine hydrate, and methanol into the reaction kettle for chemical reaction, after the reaction is completed The product is centrifuged in a centrifuge, the solid material produced is collected, the collected solid material is dissolved in water, stirred evenly and centrifuged, and the N(2)-L-alanyl-L-glutamine aqueous solution is collected;

[0041] (2) Distillation under reduced pressure: put the collected N(2)-L-alanyl-L-glutamine aqueous solution into a glass-lined reactor, close all valves of the glass-lined reactor, turn on the vacuum, and carry out vacuum distillation. During the vacuum distillation, keep the temperature in the glass-lined reactor at 60°C, the vacuum degree -0.1Mpa, and the vacuum distillation time for 2.5h; ...

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Abstract

The invention belongs to the technical field of medicine synthesis and preparation, and concretely relates to a methanol recycling method in the production process of N(2)-L-alanyl-L-glutamine. The N(2)-L-alanyl-L-glutamine is obtained through chemically reacting phthaloyl alanylglutamine and hydrazine hydrate which are used as raw materials to synthesize a product and crystallizing and purifying the product by using methanol. The method comprises the following steps: carrying out primary reduced pressure distillation on a collected aqueous solution of N(2)-L-alanyl-L-glutamine before the crystallization and purification of the N(2)-L-alanyl-L-glutamine by using the methanol in the production process in order to reduce impurities from the aqueous solution of N(2)-L-alanyl-L-glutamine, collecting waste methanol after the production process, and distilling the collected waste methanol to realize recovery and recycling. The method greatly reduces the production cost of the product and the environmental cost and the risk of the treatment of the waste methanol, and the recovered methanol can be directly used in the production process of the N(2)-L-alanyl-L-glutamine, and has no influences on the yield or the quality of the product.

Description

technical field [0001] The invention belongs to the technical field of synthesis and preparation of medicines, and in particular relates to a methanol recycling method in the production process of N(2)-L-alanyl-L-glutamine. Background technique [0002] N(2)-L-alanyl-L-glutamine (commonly known as dipeptide) is an amino acid drug and an important part of parenteral nutrition. It is suitable for patients who need to supplement glutamine, including those in Patients with catabolic and hypermetabolic conditions. Glutamine is a conditionally essential amino acid, an important precursor for the synthesis of nucleic acids, proteins, purines, pyrimidines, etc., and a regulator of protein synthesis and decomposition. However, glutamine itself cannot be directly used as a drug due to its instability and low water solubility. Converting it into N(2)-L-alanyl-L-glutamine can fully exert the effect of glutamine on the human body. [0003] At present, the conventional production proces...

Claims

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Application Information

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IPC IPC(8): C07K5/062C07K1/30C07C29/80C07C31/04
CPCC07C29/80C07K5/06026C07C31/04
Inventor李亭孙亚萍韩冉孔霞李若清
Owner山东辰龙药业有限公司