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Synthesis method of hydroxyethyl ethylenediamine

A technology of hydroxyethylethylenediamine and a synthesis method, applied in the direction of organic chemistry and the like, can solve the problems of high safety risk of ethylene oxide, waste of subsequent processing, power loss, etc. The effect of high safety

Active Publication Date: 2021-02-19
SHANDONG GUOBANG PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The ethylene oxide method is a route that has been widely studied in the industry at present, but the safety risk of ethylene oxide is high, and the reaction process of ethylenediamine and ethylene oxide is a series reaction, which is very easy to generate dihydroxyethylethylenediamine , trihydroxyethylethylenediamine or even tetrahydroxyethylethylenediamine and other byproducts, resulting in a large amount of waste and difficulties in follow-up treatment, although some literature mentions the use of gas-liquid reaction devices to reduce the generation of byproducts, but it will also bring massive loss of power

Method used

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  • Synthesis method of hydroxyethyl ethylenediamine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Take 300g (5mol) of anhydrous ethylenediamine and add it to a four-neck flask with mechanical stirring, add 15.9g (0.15mol) of anhydrous sodium carbonate as a basic catalyst, stir at 400-600rpm, and slowly add it dropwise 432g (4.8mol) methyl glycolate, control the dropping time for 6 hours, and control the temperature during the dropping process to be 25°C; after the dropping is completed, stir for 2 hours, open the vacuum system, reclaim methanol, and take samples for detection in the middle until the methanol is recovered cleanly. The material is transferred into the autoclave;

[0033] Add 600g of dioxane, put in 30g of Raney copper as a hydrogenation catalyst, tighten the lid of the kettle, replace the air three times after the nitrogen leak test, and replace it with hydrogen twice;

[0034] Turn on the stirring at 400-600rpm, raise the temperature at the same time, raise the temperature to 170°C, fill in hydrogen to keep the pressure at 5±0.5MPa, observe the chang...

Embodiment 2

[0037] What this implementation method is different from Example 1 is that the addition of alkaline catalyst anhydrous sodium carbonate is 2.65g (0.025mol), and other steps are identical, obtain 393.45g product, molar yield 91.5%, gas phase detection purity is 99.1%.

Embodiment 3

[0039] What this implementation method is different from Example 1 is that the addition of alkaline catalyst anhydrous sodium carbonate is 5.3g (0.05mol), and other steps are identical, obtain 396.89g product, molar yield 92.3%, gas phase detection purity is 99.4%.

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Abstract

The invention discloses a synthesis method of hydroxyethyl ethylenediamine, wherein the synthesis method comprises the steps: adding a basic catalyst into anhydrous ethylenediamine, slowly dropwise adding methyl glycolate, recovering an organic solvent from the obtained product under vacuum conditions, and carrying out hydrogenation reaction on a feed liquid after recovery; and after hydrogenationunder the action of a hydrogenation catalyst, filtering the obtained feed liquid to remove the hydrogenation catalyst, rectifying, and collecting the fraction to obtain the finished product hydroxyethyl ethylenediamine. The method is simple in process operation, high in conversion rate, good in selectivity, high in total yield, environment-friendly and less in three wastes, and has a good industrial prospect.

Description

technical field [0001] The invention belongs to the technical field of organic chemical industry, and also belongs to the technical field of synthesis of veterinary drugs and pharmaceutical raw materials, in particular to a method for synthesizing hydroxyethylethylenediamine. Background technique [0002] Hydroxyethylethylenediamine (piperazine) is an important chemical raw material and pharmaceutical intermediate, mainly used in the production of anthelmintic drugs piperazine phosphate, piperazine citrate, and fluphenazine, chlorpheniramine, Rifampicin. Among them, piperazine hexahydrate can also synthesize hormone drugs such as prednisolone sodium phosphate, acetylpiperazine, rubber vulcanizing agent, antioxidant, preservative, surfactant, synthetic resin, synthetic fiber, synthetic leather, etc., and has a wide range of uses. [0003] At present, there are three main routes for industrially synthesizing piperazine: the chloroethanol method, the ethanolamine method and th...

Claims

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Application Information

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IPC IPC(8): C07D295/023C07D295/027
CPCC07D295/023C07D295/027Y02P20/584
Inventor 邱正洲李芳钟志军张小垒王召平
Owner SHANDONG GUOBANG PHARMA