Preparation method of 3-dimethylamino-1,2-propanediol

A technology of dimethylamino group and propylene glycol, which is applied in the preparation of organic compounds, preparation of amino hydroxyl compounds, chemical instruments and methods, etc., can solve the problems of not meeting the requirements of drug production, poor quality, low yield, etc., and achieve The effect of significant economic benefits

Inactive Publication Date: 2015-02-25
太仓市茜泾化工有限公司
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  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

The purity of the product obtained by the traditional method is only about 90% (GC), the content of impurities is high, and the quality is poor, which cannot meet the requirements of pharmaceutical production
In addition, the yield of the traditional method is only about 70%, the yield is low, and the cost is high

Method used

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  • Preparation method of 3-dimethylamino-1,2-propanediol

Examples

Experimental program
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Embodiment 1

[0020] Put 247g of 40wt% dimethylamine aqueous solution into a 1000ml reaction bottle, add dropwise 3-chloro-1,2-propanediol methanol diluent (200g of 3-chloro-1,2-propanediol + 267ml of methanol) below 25°C, about 25% dropwise At the same time, the remaining methanol dilution of 3-chloro-1,2-propanediol and methanol dilution of sodium methoxide (sodium methoxide 345g+methanol 147ml) were added dropwise at the same time. ℃, heat preservation reaction for 3 hours, then raise the temperature to reflux, keep it for 2 hours, cool to room temperature and filter, and rinse the filter cake with an appropriate amount of methanol. The filtrates were combined, methanol was evaporated under reduced pressure, 330ml of toluene was added, the total reflux dehydration was carried out to an internal temperature above 110°C, cooled to room temperature, filtered, the toluene was evaporated under reduced pressure, and 171.9 g of the product was obtained by rectification, yield: 79.8%, The GC con...

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Abstract

The invention relates to a preparation method of 3-dimethylamino-1,2-propanediol. The preparation method is characterized in that dimethylamine and 3-chloro-1,2-propanediol are subjected to substitution reaction in a solvent in the presence of alkali to generate 3-dimethylamino-1,2-propanediol; in particular, the alkali is sodium methoxide, and the solvent is a composition of water and methanol. The method comprises the following steps: putting a dimethylamine water solution into a reactor, dropwise adding a methanol solution of 3-chloro-1,2-propanediol at 25 DEG C, simultaneously dropwise adding the remaining methanol solution of 3-chloro-1,2-propanediol and a methanol solution of sodium methoxide when the dropwise adding amount of 3-chloro-1,2-propanediol is 20-30% of the total feeding amount of 3-chloro-1,2-propanediol, after dropwise adding is finished, stirring the solution for 1-3 hours, then heating the solution to 30-40 DEG C, carrying out thermal reaction for 2-4 hours, then heating the solution till reflux, maintaining the solution for 1-3 hours, and finishing reaction. The preparation method has the advantages that the reaction conditions and the reaction processes are comprehensively design; by adopting the method, the purity and yield of the obtained product can be 99.5% and 80% respectively; the preparation method has obvious economic benefits.

Description

technical field [0001] The invention relates to a preparation method of 3-dimethylamino-1,2-propanediol. Background technique [0002] 3-Dimethylamino-1,2-propanediol (DAP) is an important chemical raw material and pharmaceutical intermediate. As a chemical raw material, DAP can be used to produce cationic waterborne polyurethane, degradable fabric softener, anion exchange resin, surfactant and catalyst, etc.; as a pharmaceutical intermediate, DAP can be used to produce anesthetics, anticancer drugs and Antibacterial agents, etc. [0003] The traditional production method of DAP is to add dimethylamine solution, 40% sodium hydroxide solution and 3-chloro-1,2-propanediol into the reactor in sequence, raise the temperature to 50℃~60℃, and stop the reaction for about 4 hours. , to obtain a light yellow liquid, first remove the remaining dimethylamine by normal pressure distillation, then remove water by distillation under reduced pressure, obtain a brownish red liquid after f...

Claims

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Application Information

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IPC IPC(8): C07C215/10C07C213/04
Inventor 洪镛裕
Owner 太仓市茜泾化工有限公司
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