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A kind of method for preparing n-methylpiperazine

A technology of methylpiperazine and methylethylenediamine, which is applied in the field of preparing N-methylpiperazine, can solve the problems such as difficulty in obtaining raw materials of diethanolamine, irritation of the respiratory tract, environmental hazards, etc., and achieves high catalytic activity and thermal stability. Stability ability, promotion of reactant conversion, low price effect

Active Publication Date: 2022-07-19
SHANDONG GUOBANG PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main disadvantage of this method is that diethanolamine is used as a raw material. Diethanolamine is a dangerous product. When people inhale diethanolamine vapor or substances, it will irritate the respiratory tract, and dizziness, coughing, vomiting, and coma may occur. The environment is harmful, and it can also cause pollution to water bodies, and the raw materials for preparing diethanolamine are not easy to obtain, etc.

Method used

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  • A kind of method for preparing n-methylpiperazine
  • A kind of method for preparing n-methylpiperazine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Prepare a 1L beaker, add 296.50g (ie 4.0mol) N-methylethylenediamine, 495.97g (ie 4.2mol) dimethyl oxalate, add 50g Raney nickel, transfer the feed liquid into a 1L reaction kettle, After 3 times of nitrogen replacement at room temperature, the reactor was leak tested, filled with hydrogen 0.15MPa for replacement, and heated to 180°C. Continue to charge hydrogen to 4.0MPa and react for 3.0h, control the temperature at 180°C. After the reaction, use circulating water to cool down to 40°C to prevent methanol from volatilizing after the reaction, stop stirring, discharge the hydrogen to the pressure of 0.01MPa, and replace with nitrogen for 3 First, to prevent residual hydrogen in the kettle, open the reactor, recover the reaction solution and catalyst in a beaker, let stand for 1 hour, let the catalyst stand at the bottom of the beaker, and take samples for analysis by gas chromatography.

[0020] The results of gas chromatography analysis showed that the conversion rate ...

Embodiment 2

[0022] Prepare a 1L beaker, add 296.50g (ie 4.0mol) N-methylethylenediamine, 495.97g (ie 4.2mol) dimethyl oxalate, add 50g Raney nickel, transfer the feed liquid into a 1L reaction kettle, After 3 times of nitrogen replacement at room temperature, the reaction kettle was tested for leaks, stirred and mixed evenly, filled with hydrogen at 0.15MPa for replacement, and heated to 150°C. Continue to charge hydrogen to 4.0MPa, react for 3.0h, control the temperature at 150°C, use circulating water to cool down to 40°C, stop stirring, discharge the hydrogen to the pressure of 0.01MPa in the kettle, and replace it with nitrogen for 3 times, then open the reaction kettle and recover the reaction solution. Put the catalyst and the catalyst in a beaker, let stand for 1 hour, let the catalyst stand at the bottom of the beaker, and take a sample for analysis by gas chromatography.

[0023] The results of gas chromatography analysis showed that the conversion rate of N-methylethylenediamine...

Embodiment 3

[0025] Prepare a 1L beaker, add 296.50g (ie 4.0mol) N-methylethylenediamine, 495.97g (ie 4.2mol) dimethyl oxalate, add 50g Raney nickel, transfer the feed liquid into a 1L reaction kettle, After 3 times of nitrogen replacement at room temperature, the reaction kettle was tested for leaks, stirred and mixed evenly, filled with hydrogen 0.15MPa for replacement, and heated to 200°C. Continue to charge hydrogen to 4.0MPa, react for 3.0h, control the temperature at 200°C, use circulating water to cool down to 40°C, stop stirring, discharge the hydrogen to the pressure of 0.01MPa in the kettle, replace with nitrogen three times, open the reactor, and recover the reaction solution Put the catalyst and the catalyst in a beaker, let stand for 1 hour, let the catalyst stand at the bottom of the beaker, and take a sample for analysis by gas chromatography.

[0026] The results of gas chromatography analysis showed that the conversion rate of N-methylethylenediamine was 96.45%, the select...

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Abstract

The invention provides a method for preparing N-methylpiperazine, which solves the problem that the existing method for preparing N-methylpiperazine uses diethanolamine, a dangerous product, as a raw material, which is harmful to human health and the environment, and the raw material for preparing diethanolamine is not easy. Technical problems such as obtaining, the preparation method includes ester aminolysis reaction and hydrogenation reduction reaction, namely, dimethyl oxalate and N-methylethylenediamine undergo aminolysis reaction to generate lactam; and then use the lactam as a reactant , adding catalyst Raney nickel, at a temperature of 150-200 ° C and a pressure of 3.0-5.0 MPa, hydrogen is introduced to carry out hydrogenation reduction reaction, and finally the N-methylpiperazine is obtained, which can be widely used in chemical materials technical field.

Description

technical field [0001] The present application relates to the technical field of chemical materials, in particular to a method for preparing N-methylpiperazine. Background technique [0002] N-methylpiperazine is an important organic chemical intermediate, which has a wide range of applications in the fields of medicine, pesticides, plastics, rubber and other chemical industries. In the field of medicine, N-methylpiperazine is an intermediate of a new generation of broad-spectrum antibacterial drugs ofloxacin and clozapine, mainly used for the synthesis of quinolone antibacterial drugs such as ofloxacin, levofloxacin, fleroxacin, perflu Floxacin, loguanfloxacin, rufloxacin, etc. Using N-methylpiperazine as raw material, it can also synthesize anti-AIDS drugs, anti-rheumatic drugs and be used as important intermediates of pesticides. In addition, N-methylpiperazine is also widely used as a selective solvent and surfactant for extracting aromatic hydrocarbons from hydrocarbo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D295/023C07D295/03
CPCC07D295/023C07D295/03
Inventor 廖仕学张越刘聪潘燕朋孙玫
Owner SHANDONG GUOBANG PHARMA
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