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High-pressure synthesis method for metronidazole

A technology of high-pressure synthesis and metronidazole, applied in organic chemistry and other fields, can solve the problem of low utilization rate of ethylene oxide, achieve the effect of improving utilization rate and reducing pollution

Inactive Publication Date: 2018-06-26
曾舟华
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the above three patents have increased the chance of contact reaction between ethylene oxide and materials to varying degrees, since they all react in an open system at normal pressure, there is still a large amount of ethylene oxide that has no time to react and is discharged as tail gas Outside the kettle, so that the utilization rate of ethylene oxide is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] 1) In the pressure-resistant reactor, drop into nitrate 150kg, formic acid 105kg and sulfuric acid 95kg;

[0016] 2) After cleaning and checking the pressure safety valve, cover the sealed kettle cover;

[0017] 3) Set the control pressure value (gauge pressure) to 1.013×10 6 Pa;

[0018] 4) Slowly feed 54 kg of ethylene oxide to the bottom of the pressure-resistant reactor. When the temperature and pressure rise rapidly, reduce the amount of ethylene oxide introduced. When the pressure is close to the pressure control value, further reduce or suspend The amount of ethylene oxide fed, when the temperature is low and the pressure is far away from the control pressure value, slightly increase the amount of ethylene oxide fed;

[0019] 5) After passing through, keep warm at 89-93°C, react for 1-12 hours, and separate the metronidazole product.

Embodiment 2

[0021] 1) In the pressure-resistant reactor, drop into nitrate 150kg, formic acid 105kg and sulfuric acid 95kg;

[0022] 2) After cleaning and checking the pressure safety valve, cover the sealed kettle lid, and replace the air above the solution in the pressure-resistant reactor with ethylene oxide;

[0023] 3) Set the control pressure value (gauge pressure) to 0.5×10 5 Pa;

[0024] 4) stirring;

[0025] 5) Slowly feed 54 kg of ethylene oxide to the bottom of the pressure-resistant reactor. When the temperature and pressure rise rapidly, reduce the amount of ethylene oxide introduced. When the pressure is close to the control pressure value, further reduce or pause The amount of ethylene oxide fed, when the temperature is low and the pressure is far away from the control pressure value, slightly increase the amount of ethylene oxide fed;

[0026] 6) After passing through, keep warm at 89-93°C, react for 1-12 hours, and separate the metronidazole product.

Embodiment 3

[0028] 1) In the pressure-resistant reactor, drop into nitrate 150kg, formic acid 105kg and sulfuric acid 95kg;

[0029] 2) After cleaning and checking the pressure safety valve, cover the sealed kettle cover;

[0030] 3) Set the control pressure value (gauge pressure) to 1.013×10 5 Pa;

[0031] 4) stirring;

[0032] 5) Slowly feed 54 kg of ethylene oxide to the bottom of the pressure-resistant reactor. When the temperature and pressure rise rapidly, reduce the amount of ethylene oxide introduced. When the pressure is close to the control pressure value, further reduce or pause The amount of ethylene oxide fed, when the temperature is low and the pressure is far away from the control pressure value, slightly increase the amount of ethylene oxide fed;

[0033] 6) After passing through, keep warm at 89-93°C, react for 1-12 hours, and separate the metronidazole product.

[0034] In the above three embodiments, the yield of metronidazole is higher than that of the current proc...

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PUM

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Abstract

The invention discloses a high-pressure synthesis method for metronidazole, and solves the problem of a low utilization rate of ethylene oxide in the prior art. The method is characterized in that thecharacteristic that the ethylene oxide is more easily dissolved into a mixed acid solvent at higher pressure is utilized, a metronidazole synthesis reaction is performed in a closed system with pressure, and the ethylene oxide above the liquid level is dissolved into a solution to participate in the reaction. The method provided by the invention has the beneficial effects that the utilization rate of the ethylene oxide is improved, and pollution of the ethylene oxide to the environment is reduced.

Description

1. Technical field [0001] The invention belongs to the fields of organic synthesis, resource recovery and environmental protection, and particularly relates to a method for synthesizing metronidazole under high pressure. 2. Background technology [0002] Metronidazole is white or yellowish crystal or crystalline powder, used for the treatment of intestinal and parenteral amoebiasis (such as amebic liver abscess, pleural amoebiasis, etc.). It can also be used to treat vaginal trichomoniasis, cylindrosis, skin leishmaniasis, and guinea worm infection. At present, it is also widely used in the treatment of anaerobic infection, and is regarded as the drug of choice for anti-anaerobic bacteria by the World Health Organization (WHO). [0003] The synthesis of metronidazole takes the mixed acid of formic acid and sulfuric acid as the solvent, 2-methyl-5-nitroimidazole as the precursor compound, and ethylene oxide as the hydroxylating agent. Since the boiling point of ethylene oxi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D233/94
CPCC07D233/94
Inventor 曾舟华黄刚明曾彩红黄林勇杨水彬
Owner 曾舟华
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