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Preparation method of N,N-dimethylglycine

A technology of dimethylglycine and dimethylglycine salt, which is applied in the chemical industry, can solve problems such as application limitations, and achieve the effects of high production efficiency, reduced production costs, and simple post-processing

Active Publication Date: 2013-11-13
CHONGQING UNISPLENDOUR CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method has become the mainstream process for the preparation of N,N-dimethylglycine, the hydrochloride of N,N-dimethylglycine is obtained, and its application is still limited.

Method used

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  • Preparation method of N,N-dimethylglycine
  • Preparation method of N,N-dimethylglycine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Embodiment 1 hydroxyacetonitrile method prepares N, N-dimethylglycine

[0042] At room temperature, add 1000g of 40% hydroxyacetonitrile aqueous solution to the high-pressure reactor, then pass through 1435g of 33% dimethylamine aqueous solution, heat up to 60°C, pressure 0.7MPa, after 0.5 hours of reaction, stop the reaction, and transfer the reaction solution to 3000ml In the flask, add 561g of 50% sodium hydroxide aqueous solution to the reaction solution, and keep it warm at 80°C for 5 hours to obtain an ammonia solution of N,N-dimethylglycine sodium salt, and deamination to obtain N,N-dimethylglycine Sodium salt solution, followed by adding 98% sulfuric acid to adjust the pH to 5.0 to obtain a mixture of N,N-dimethylglycine and sodium sulfate. Add 8g of activated carbon for decolorization, remove the activated carbon by suction filtration, cool the filtrate to 10°C, crystallize, centrifuge to remove sodium sulfate crystals, and crystallize and purify the filtrate a...

Embodiment 2

[0043] Embodiment 2 hydroxyacetonitrile method prepares N, N-dimethylglycine

[0044] At room temperature, add 1000g of 40% hydroxyacetonitrile aqueous solution to the high-pressure reactor, then pass through 1435g of 33% dimethylamine aqueous solution, heat up to 60°C, pressure 0.7MPa, after 0.5 hours of reaction, stop the reaction, and transfer the reaction solution to 3000ml In the flask, add 786g of 50% potassium hydroxide aqueous solution to the reaction solution, and keep it warm at 80°C for 5 hours to obtain an ammonia solution of N,N-dimethylglycine potassium salt, and deamination to obtain N,N-dimethylglycine Potassium salt solution, followed by adding 37% hydrochloric acid to adjust the pH to 5.0 to obtain a mixture of N,N-dimethylglycine and potassium chloride. Add 7g of activated carbon for decolorization, remove the activated carbon by suction filtration, cool the filtrate to 10°C, crystallize, centrifuge to remove potassium chloride crystals, and crystallize and ...

Embodiment 3

[0045] Embodiment 3 hydroxyacetonitrile method prepares N, N-dimethylglycine

[0046] At room temperature, add 1000g of 40% aqueous solution of hydroxyacetonitrile to the high-pressure reactor, then pass through 1435g of 33% aqueous solution of dimethylamine, raise the temperature to 60°C, and pressurize at 0.6MPa. After reacting for 0.5 hours, stop the reaction, and transfer the reaction solution into a In the flask, add an aqueous solution composed of 497g of sodium sulfate and 259g of calcium hydroxide to the reaction solution, and incubate at 85°C for 7 hours to obtain an ammonia solution of N,N-dimethylglycine sodium salt, and deamination to obtain N,N- Dimethylglycine sodium salt solution, followed by adding 37% hydrochloric acid to adjust the pH to 4.5, to obtain a mixed solution of N,N-dimethylglycine, sodium chloride and calcium sulfate. Add 8g of activated carbon for decolorization, remove the activated carbon by suction filtration, cool the filtrate to 10°C, crystal...

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Abstract

The invention relates to a preparation method of N,N-dimethylglycine and belongs to the field of chemical engineering. The preparation method comprises the following steps of: preparing N,N-dimethyl amino acetonitrile by taking hydroxyacetonitrile and dimethylamine as raw materials, obtaining an N,N-dimethylglycine crude product by alkalizing the reaction liquid with an inorganic base and neutralizing the reaction liquid with an organic acid on the basis of N,N-dimethyl amino acetonitrile reaction liquid, and finally separating and purifying the N,N-dimethylglycine crude product to obtain the high-quality N,N-dimethylglycine product. The preparation method has the advantages that the raw materials are environmentally-friendly and easily available, reaction conditions are mild, the environmental pollution is little, the after-treatment is simple and easy, the production efficiency is high, and the preparation method is suitable for industrial popularization and application.

Description

technical field [0001] The invention aims at the field of chemical industry and relates to a method for preparing N,N-dimethylglycine, in particular to a method for preparing N,N-dimethylglycine by using N,N-dimethylaminoacetonitrile. Background technique [0002] N, N-dimethylglycine (Dimethylglycine, N, N-dimethylglycine, referred to as DMG, vitamin B16), the appearance of white crystals, soluble in water and ethanol. As a drug, it can be used to treat middle-aged and elderly depression, stimulate the human immune response, reduce the damage of pollution pollutants to the body, and reduce the cholesterol content in the body. In addition, it can be used as an antioxidant in the food industry, as a pharmaceutical intermediate in the pharmaceutical industry, and to synthesize a variety of biochemical drugs. [0003] Patent US4968839 reports the synthesis process of N,N-dimethylglycine, that is, the reaction of dimethylamine with formaldehyde, sodium cyanide and sodium bisulf...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C255/25C07C253/30C07C229/12C07C227/18
Inventor 吴传隆丁永良秦岭杨帆何咏梅朱丽利任星宇
Owner CHONGQING UNISPLENDOUR CHEM
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