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N,N-dimethylglycine hydrochloride preparation method suitable for industrial production

A technology of dimethylglycine hydrochloride and dimethylamine, which is applied in the field of preparation of N,N-dimethylglycine hydrochloride, can solve the problems of many reaction by-products, expensive raw materials, and high cost, and achieve production The effect of simple process, high product purity and easy operation

Active Publication Date: 2013-12-25
山东祥维斯生物科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0015] Among the above methods, 1) the raw materials are expensive, there are many reaction by-products, the reaction conditions are not easy to control, and the yield is not high; 2) it is not suitable to extract products from the formic acid system, and industrialization is difficult; 3) the catalyst is expensive; 4) using Highly toxic sodium cyanide is used as a reaction raw material, because sodium cyanide cannot be completely reacted or hydrolyzed in the reaction, it will have an impact on the environment, and the above methods have defects, are not suitable for industrial production, and have no industrial development value; 5) Raw materials are easy to obtain, most suitable for industrial production, but need to use electrodialysis to desalinate, the cost is too high

Method used

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  • N,N-dimethylglycine hydrochloride preparation method suitable for industrial production
  • N,N-dimethylglycine hydrochloride preparation method suitable for industrial production
  • N,N-dimethylglycine hydrochloride preparation method suitable for industrial production

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Put 195kg of ethanol into the autoclave, start stirring, then add 200kg of solid chloroacetic acid (content 97.5wt%, the mass of pure chloroacetic acid is 195kg), 3.9kg of sodium iodide, after the solid chloroacetic acid dissolves, slowly pass it into the dry Dimethylamine gas is 93.02kg, and the reaction pressure is guaranteed to be 0.6MPa. After passing through, the temperature is controlled at 65°C, and the reaction is carried out for 4 hours. After the reaction is completed, the temperature is lowered to 25°C to release the pressure, and at the same time, unreacted dimethylamine is collected. After the dimethylamine was drained, the heated material was concentrated in vacuum, and ethanol was recovered. After white crystals were precipitated from the feed liquid, the concentration was stopped, and the temperature was lowered to 25°C, centrifuged, and dried to obtain 267.3kg of the product, with a content of 98.8% and a yield of 92.8%. The filtrate is set into the mate...

Embodiment 2

[0033] Put 292.5kg of dichloromethane into the autoclave, start stirring, then add 200kg of solid chloroacetic acid (content 97.5wt%, the mass of pure chloroacetic acid is 195kg), 7.8kg of sodium iodide, after the chloroacetic acid is dissolved, slowly pass in Dry dimethylamine gas 111.6kg, ensure the reaction pressure is 0.5MPa, pass through, control the temperature at 75 ° C, react for 6 hours, after the reaction is completed, the temperature will be lowered to 25 ° C to release the pressure, while collecting unreacted dimethylamine. After the dimethylamine is discharged, the heated material is concentrated in vacuum, and dichloromethane is recovered. After white crystals are precipitated from the material liquid, the concentration is stopped, the temperature is lowered to 25°C, centrifuged, and dried to obtain 269.2kg of the product, with a content of 99.3% and a yield of 93.5%. Apply the filtrate.

Embodiment 3

[0035] Put 220kg of isopropanol into the autoclave, start stirring, then add 200kg of solid chloroacetic acid (the content is 97.5wt%, the mass of pure chloroacetic acid is 195kg), 6kg of sodium iodide, after the chloroacetic acid dissolves, slowly pass it into the dry Dimethylamine gas is 94.2kg, and the reaction pressure is guaranteed to be 0.4MPa. After passing through, the temperature is controlled at 70°C, and the reaction is carried out for 5h. After the reaction is completed, the temperature is lowered to 25°C to release the pressure, and the unreacted dimethylamine is collected at the same time. After the dimethylamine was drained, the heated material was concentrated in vacuum, and isopropanol was recovered. After white crystals were precipitated from the material liquid, the concentration was stopped, and the temperature was lowered to 25°C, centrifuged, and dried to obtain 272.8kg of the product, with a content of 99.5% and a yield of 94.7%. Apply the filtrate.

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Abstract

The invention discloses an N,N-dimethylglycine hydrochloride preparation method suitable for industrial production. The N,N-dimethylglycine hydrochloride preparation method comprises the following steps of putting an organic solvent into an autoclave, adding chloroacetic acid into the organic solvent, carrying out stirring until full dissolution of chloroacetic acid, adding sodium iodide as a catalyst into the solution, slowly feeding dry dimethylamine gas into the mixed solution, carrying out a reaction process under reaction pressure of 0.3-0.7MPa at a temperature of 65-75 DEG C for 4-6h, and carrying out condensation, cooling crystallization, centrifugation and drying to obtain N,N-dimethylglycine hydrochloride. The N,N-dimethylglycine hydrochloride preparation method has simple processes, is convenient for operation, realizes high product purity, has a high yield and is suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation method of a pharmaceutical intermediate, in particular to a preparation method of N,N-dimethylglycine hydrochloride suitable for industrial production. Background technique [0002] The molecular formula of N,N-dimethylglycine hydrochloride is C4H9NO2·HCl. It is easily soluble in water and ethanol, and its aqueous solution is acidic. N,N-Dimethylglycine hydrochloride is widely used as a raw material for medicine and health care products. As a medicine, it can be used to treat depression, improve the immunity of the human body, and enhance the tolerance of the human body. The methyl group in the structure has the function of transmethylation, which can be used to resist tumors and cancers, and can be widely used in the synthesis of anticancer drugs. N,N-Dimethylglycine hydrochloride can be used as a skin penetration enhancer and cosmetic additive due to its strong water absorption. [0003] In the past, the meth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C229/12C07C227/08
Inventor 马兴群张守伟丁振柱张毅丰曾凡伟
Owner 山东祥维斯生物科技股份有限公司
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