Process for synthesizing N-ethyl piperazidine

A synthesis method and technology of ethylpiperazine are applied in the synthesis field of N-ethylpiperazine, and can solve the problems of process control, difficult three-waste treatment, many by-products, and many reaction steps, etc. demanding effects

Active Publication Date: 2010-05-19
ZHEJIANG XINHUA CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that the reaction temperature is high, resulting in high equipment requirements; there are many reaction steps and equipment and instruments, resulting in great difficulty in process control and three waste treatment; poor catalyst selectivity, low conversion rate, and many by-products

Method used

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  • Process for synthesizing N-ethyl piperazidine

Examples

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Comparison scheme
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Embodiment 1

[0010] Embodiment 1: adjust the high-speed stirrer, measuring (controlling) temperature system, pressure gauge, safety valve etc. of 5L stainless steel autoclave, and replace the autoclave with nitrogen to 0 2 ≤0.5%, add 260 grams of anhydrous piperazine (purity 99.5%), 4.5 grams of 1# catalyst, and 46 grams of anhydrous alcohol at one time, wherein the composition of 1# catalyst (wt%): Cu: 1.0%, Co: 1.0 %, Mo: 2.5%, Ni: 1.0%, Mn: 0.5%, Mg: 0.1%, Cr: 0.05%, and the rest is Al 2 O 3 . After the replacement with hydrogen is qualified, the pressure in the kettle is raised to 3.0 MPa with hydrogen, and the hydrogenation valve is closed. Start stirring and heating, the temperature is controlled at 190-210 ° C, and the ammonia pressure is controlled within 6.0 MPa. During the reaction, the temperature will rise significantly, and the heat of reaction should be removed in time. The reaction was carried out for 3 hours, the temperature was lowered, the pressure was relieved, the r...

Embodiment 2

[0011] Example 2: Add 85 grams of anhydrous piperazine, and the others are the same as in Example 1.

Embodiment 3

[0012] Example 3: add 420 g of anhydrous piperazine, react for 2 hours, and the others are the same as in Example 1.

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Abstract

The invention discloses a synthesizing method of N-ethyl piperazine, which comprises the following steps: adopting Cu-Co-M0 / Al2O3 as catalyst with 1-70% Cu, 1-90% Co,1-30% Mo, 0.1-10% Ni, 0.05-10% Mn, 0.01-5.0% Mg, 0.01-5.0% Cr and Al2O3; setting the pressure of liquid phase at 0.1-10.0Mpa under 80-350 Deg C in the interval course with surplus piperazidine; making the molar rate of piperazidineand alcohol at 0.5-10.0 with 0.1-5.0% catalytic cracking quantity.

Description

technical field [0001] The invention relates to a chemical synthesis method, in particular to a synthesis method of N-ethylpiperazine using ethanol and piperazine as raw materials. Background technique [0002] N-Ethylpiperazine is one of the piperazine series products. It is an important fine chemical and an intermediate for the synthesis of medicines and pesticides. It is mainly used for the synthesis of ethyl ciprofloxacin antibacterial drugs. It is used as a synthetic raw material for products such as dyes and plant protection agents, and is also widely used in fungicides and surfactants. The product is still in the development stage in China, and its consumption mainly depends on imports. There are two main synthetic methods known in the literature: [0003] Method 1: Synthesis with piperazine as raw material: prepared by reacting piperazine with acetonitrile, acetaldehyde or bromoethane. The method for synthesizing N-ethylpiperazine by the reaction of piperazine and...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D295/03B01J23/885
Inventor 陈国建谢自强刘训军
Owner ZHEJIANG XINHUA CHEM
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