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A kind of synthetic method of n-ethyl-2,3-dioxypiperazine

A synthetic method, the technology of dioxypiperazine, applied in the direction of organic chemistry, etc., can solve the problems such as the difficulty of controlling the amount of ammonium chloride, the impact of product yield and quality, and side reactions

Active Publication Date: 2020-10-27
石家庄金派医药化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Specifically in the ring closure process, two methods are generally used to promote the reaction: the first is to feed a sufficient amount of carbon dioxide as a catalyst, but in the process of operation, the speed and amount of carbon dioxide gas are difficult to pass. Accurate control, and the reaction process is a gas-liquid two-phase, which makes the reaction cycle long, the process controllability is poor, the energy consumption is high, and the safety hazard is large, which is not conducive to industrial production
The second is to add solid ammonium chloride as a catalyst. Although the reaction conditions have been greatly improved compared with passing carbon dioxide, the solubility of solid ammonium chloride in the material is not high, and ammonium chloride is easily mixed with the commonly used cyclizing agent oxalic acid di Ethyl ester has a side reaction, because the addition of ammonium chloride is not easy to grasp, thereby affecting the yield and quality of the product
For the purification problem of product, in known method, two kinds of solvents such as ethyl acetate and isopropanol or ethyl acetate and ethanol are generally used in combination, which causes a lot of troubles for the recovery and secondary use of the solvent. Not conducive to industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Embodiment 1 The synthetic method of N-ethyl-2,3-dioxypiperazine of the present invention

[0018] a. Add 11g of N-ethylethylenediamine to 10g of anhydrous methanol to form a mixed solution A;

[0019] b. Add 25ml of anhydrous methanol into a dry three-necked flask, add 0.2g of ammonium chloride under stirring, and stir to dissolve completely, then add 19g of diethyl oxalate at 25-30°C, cool down to 15-20°C, and stir well. Put it in the dropping funnel to get the mixed solution B;

[0020] c. Add the mixed solution A dropwise to the mixed solution B in 30 to 50 minutes. After completion, raise the temperature to 50°C and keep it warm for 1 hour. After the reaction is completed, use the method of concentration under reduced pressure to distill out the methanol;

[0021] d. Add 55ml of ethylene glycol dimethyl ether, and the material is placed at room temperature (25-30°C) at 50°C for slow crystallization to obtain the target product N-ethyl-2,3-dioxypiperazine 14.43g (y...

Embodiment 2

[0022] Embodiment 2 The synthetic method of N-ethyl-2,3-dioxypiperazine of the present invention

[0023] a. Add 11g of N-ethylethylenediamine to 8g of anhydrous methanol to form a mixed solution A;

[0024] b. Add 25ml of anhydrous methanol into a dry there-necked flask, add 2g of glacial acetic acid while stirring, and stir to dissolve completely, then add 11g of diethyl oxalate at 25-30°C, cool down to 15-20°C, stir well, and place In the dropping funnel, mixed solution B was obtained;

[0025] c. Add the mixed solution A dropwise to the mixed solution B in 30 to 50 minutes. After completion, raise the temperature to 50°C and keep it warm for 1 hour. After the reaction is completed, use the method of concentration under reduced pressure to distill out the methanol;

[0026] d. Add 66ml of ethylene glycol dimethyl ether, and the material is placed at room temperature (25-30°C) at 50°C for slow crystallization to obtain 14.77g of the target product N-ethyl-2,3-dioxypiperazin...

Embodiment 3

[0027] Embodiment 3 The synthetic method of N-ethyl-2,3-dioxypiperazine of the present invention

[0028] a. Add 11g of N-ethylethylenediamine to 11g of anhydrous methanol to form a mixed solution A;

[0029] b. Add 25ml of anhydrous methanol into a dry three-necked flask, add 2g of glacial acetic acid while stirring, and stir to dissolve completely, then add 19g of diethyl oxalate at 25-30°C, cool down to 15-20°C, stir well, and place In the dropping funnel, mixed solution B was obtained;

[0030] c. Add the mixed solution A dropwise to the mixed solution B in 30 to 50 minutes. After completion, raise the temperature to 50°C and keep it warm for 1 hour. After the reaction is completed, use the method of concentration under reduced pressure to distill out the methanol;

[0031] d. Add 44ml of ethylene glycol dimethyl ether, and the material is placed at room temperature (25-30°C) at 50°C for slow crystallization to obtain 12.81g of the target product N-ethyl-2,3-dioxypiperazi...

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PUM

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Abstract

The invention relates to a synthetic method of N-ethyl-2,3-dioxygen piperazine, belonging to the technical fields of pharmaceutical and chemical industry. The synthetic method comprises the steps of preparing a mixed solution A from N-ethyl ethanediamine and absolute methanol, adding a catalyst and diethyl oxalate into absolute methanol, and uniformly stirring, so as to obtain a solution B. Compared with the prior art, the synthetic method of N-ethyl-2,3-dioxygen piperazine has the advantages that the raw materials are easily available, the operation is simple, conditions are mild, the quality is stable, and the energy consumption is low; and the synthetic method is environment-friendly and has very good industrial prospects and promotional values.

Description

technical field [0001] The invention relates to a compound synthesis method, in particular to a synthesis method of N-ethyl-2,3-dioxypiperazine, which belongs to the technical field of medicine and chemical industry. Background technique [0002] N-ethyl-2,3-dioxypiperazine is an important intermediate for the preparation of piperacillin, cefoperazone, cefoperazone and other types of compounds. With the continuous advancement of pharmaceutical and chemical technology and the rapid growth of the antibiotic market, the pharmaceutical and chemical research and development personnel of each unit are constantly striving to innovate or improve the existing process route, making its products more economical and environmentally friendly, and the process conditions are simpler and more convenient. Continuously improve the efficiency and promote the long-term development of the enterprise. [0003] Among the methods disclosed in existing materials: the preparation of N-ethyl-2,3-diox...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D241/08
CPCC07D241/08
Inventor 李九军李娜
Owner 石家庄金派医药化工有限公司
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