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Preparation method of high-purity glycine methyl ester hydrochloride

A technology of hydrochloride and amino acid ester is applied in the fields of low temperature, the preparation of similar glycine ester hydrochloride, and the preparation of high-purity amino acid methyl ester hydrochloride, which can solve problems that are not conducive to industrialization promotion, personal safety and environmental friendliness. , increase the production cost of products, etc., to achieve the effect of easy industrial production, good crystal form, and easy control of crystallization

Inactive Publication Date: 2019-07-12
SHANDONG TAIHE WATER TREATMENT TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Extensive use of low-boiling organic solvents in the crystallization process in the existing technology is not conducive to personal safety and environmental friendliness, and increases the production cost of the product, which is not conducive to industrialization

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] (1) At room temperature, add 150g of glycine and 640g of anhydrous methanol (among them: the molar ratio of glycine to anhydrous methanol is 1:10) into the reactor with stirring, start stirring to mix evenly;

[0018] (2) Infuse hydrogen chloride gas at a flow rate of 40L / h for 20 minutes until the system is completely dissolved, and at the same time raise the reaction temperature of the system to 45±1°C;

[0019] (3) When the heat preservation reaction lasts for 0.75 hours until crystals are precipitated in the system, continue to feed hydrogen chloride gas at a flow rate of 30L / h;

[0020] (4) Control the stirring rate to 120r / min, and the system drops to ≤10°C according to the gradient of 4°C / h;

[0021] (5) After suction filtration and drying at 100±5°C for 2 hours, a total of 241.58g of white crystal fine granular glycine methyl ester hydrochloride was obtained, and the yield was 95.64% based on the amount of glycine fed; the NMR purity of the product was 99.37% af...

Embodiment 2

[0023] (1) At room temperature, add 150g of glycine and 512g of anhydrous methanol (among them: the molar ratio of glycine to anhydrous methanol is 1:8) into the reactor with stirring, and start stirring to mix evenly;

[0024] (2) Infuse hydrogen chloride gas at a flow rate of 30L / h for about 30 minutes until the system is completely dissolved, and at the same time raise the reaction temperature of the system to 55±1°C;

[0025] (3) Insulate and react for 0.5 hours, and continue to feed hydrogen chloride gas at a flow rate of 20L / h until crystals are precipitated in the system;

[0026] (4) Control the stirring rate to 240r / min, and the system drops to ≤10°C according to the gradient of 4°C / h;

[0027] (5) After suction filtration and drying at 100±5°C for 2 hours, a total of 238.02g of glycine methyl ester hydrochloride in the form of white crystals and fine particles was obtained, and the yield was 93.90% based on the amount of glycine fed; the purity of the product was tes...

Embodiment 3

[0029] Control the agitation rate of late crystallization to 180r / min, the system drops to room temperature according to the gradient of 6°C / h, and other process conditions and operating procedures are the same as in Example 1.

[0030] After suction filtration and drying, a total of 241.30g of white crystal fine granular glycine methyl ester hydrochloride was obtained, and the product yield was 95.29%; the purity of the product was tested to be 99.12%, the melting point of the product was 173.1-173.3°C, and the content of glycine hydrochloride was 0.64%. After filtration, the methanol-containing mother liquor is recycled for the synthesis reaction of glycine methyl ester hydrochloride.

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Abstract

A preparation method of high-purity glycine methyl ester hydrochloride specifically comprises the steps that 1, glycine and absolute methanol are added into a reaction kettle and uniformly stirred andmixed; 2, hydrogen chloride gas is introduced, and the reaction temperature of a system is increased to be 40-60 DEG C; 3, hydrogen chloride gas is continuously introduced for 0-20 minutes when crystal is separated out in the system due to a thermal reaction; 4, the stirring rate is controlled and gradiently reduced until the temperature of the system is lower than or equal to 10 DEG C, and suction filtration and drying are carried out to obtain the white crystalline powder glycine methyl ester hydrochloride. According to the method, the glycine and the absolute methanol serve as raw materials, the introducing amount and introducing stage of the hydrogen chloride gas are controlled, and amino acid methyl ester hydrochloride with the purity higher than 99% is prepared at a time through a gradient cooling crystallization method, so that the problems of instant crystallization of the solvent-free reaction system, equipment stirring locking, high filtration energy consumption and the likeare effectively solved. According to the method, the reaction equipment is simple, reaction conditions are mild, crystallization is easy to control, and the product yield can reach 95%.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a method for preparing low-temperature, high-purity amino acid methyl ester hydrochloride, and the method is also applicable to the preparation of similar glycine ester hydrochloride. Background technique [0002] Glycine methyl ester hydrochloride is a white crystalline powder at room temperature, easily soluble in water, slightly soluble in ethanol, easy to absorb moisture when placed in the air. Glycine methyl ester hydrochloride can be used for the treatment of sivelestat sodium for acute lung injury caused by systemic inflammatory response syndrome, long-acting angiotensin II receptor antagonist irbesartan, for the treatment of atherosclerosis It is an important pharmaceutical intermediate for the synthesis of various drugs such as sclerosis. [0003] There are two main synthesis methods of glycine methyl ester hydrochloride: one is to synthesize glycine with chloroacetic a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C227/18C07C227/42C07C229/08
CPCC07C227/18C07C227/42C07C229/08
Inventor 王宁宁程终发齐晓婧陆久田刘全华
Owner SHANDONG TAIHE WATER TREATMENT TECH CO LTD
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