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Metronidazole production method

A technology for metronidazole and nitroimidazole, applied in the direction of organic chemistry and the like, can solve the problems of large alkali consumption, high cost, large waste water discharge, etc., and achieves reduction of alkali usage, improvement of yield, and reduction of production costs. Effect

Active Publication Date: 2014-01-01
HUBEI HONGYUAN PHARMA
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] One of the purposes of the present invention is to solve the problems of large amount of alkali consumption, large waste water discharge and high cost when preparing metronidazole by the existing formic acid method; the second purpose of the present invention is to improve the quality of metronidazole by reasonably controlling the reaction process and reaction parameters. Yield of azole

Method used

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Effect test

Embodiment 1

[0032] (1) Preparation of mixed acid: put 270kg of formic acid with a mass concentration of 85% into a hydroxylation reaction kettle, and add 160kg of concentrated sulfuric acid with a mass concentration of 98% while stirring at a temperature of 18°C ​​to prepare a mixed acid.

[0033] (2) Hydroxylation reaction: Put 400kg of 2-methyl-5-nitroimidazole into the hydroxylation reaction kettle equipped with mixed acid, stir and heat up to 80°C, after 2-methyl-5-nitroimidazole is completely dissolved Insulate for 15 minutes, then add 260kg of ethylene oxide and 55kg of 98wt% concentrated sulfuric acid alternately in 240 minutes, and generate hydroxylated liquid after the reaction is completed.

[0034] (3) Recovery of formic acid: transfer the hydroxylated solution obtained in step (2) into a still, control the temperature at 65°C, control the vacuum degree to -0.086MPa, and distill under reduced pressure, the distillate is formic acid.

[0035] (4) Neutralization: transfer the cen...

Embodiment 2

[0040] (1) Preparation of mixed acid: Put 270kg of formic acid with a mass concentration of 90% into a hydroxylation reaction kettle, add 180kg of 98wt% concentrated sulfuric acid while stirring at a temperature of 25°C to prepare a mixed acid.

[0041] (2) Hydroxylation reaction: Put 430kg of 2-methyl-5-nitroimidazole into the hydroxylation reaction kettle equipped with mixed acid, stir and heat up to 88°C, after 2-methyl-5-nitroimidazole is completely dissolved Keep warm for 10 minutes, then add 270kg of ethylene oxide and 60kg of 98wt% concentrated sulfuric acid alternately in 300 minutes, and generate hydroxylated solution after the reaction is completed.

[0042] (3) Recovery of formic acid: transfer the hydroxylated solution obtained in step (2) into a still, control the temperature at 80°C, control the vacuum degree to -0.085MPa, and distill under reduced pressure, the distillate is formic acid.

[0043] (4) Neutralization: Transfer the centrifuged mother liquor obtaine...

Embodiment 3

[0048] (1) Preparation of mixed acid: put 270kg of formic acid with a mass concentration of 88% into the hydroxylation reaction kettle, and add 170kg of 98wt% concentrated sulfuric acid while stirring at a temperature of 32°C to prepare the mixed acid.

[0049] (2) Hydroxylation reaction: Put 420kg of 2-methyl-5-nitroimidazole into the hydroxylation reaction kettle equipped with mixed acid, stir and heat up to 85°C, after 2-methyl-5-nitroimidazole is completely dissolved Insulate for 12 minutes, then add 265kg of ethylene oxide and 56kg of 98wt% concentrated sulfuric acid alternately in 270 minutes, and generate hydroxylated liquid after the reaction is completed.

[0050] (3) Recovery of formic acid: transfer the hydroxylated liquid obtained in step (2) into a distillation kettle, control the temperature at 85°C, control the vacuum degree to -0.090MPa, and distill under reduced pressure, the distillate is formic acid.

[0051] (4) Neutralization: transfer the centrifuged moth...

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Abstract

The invention discloses a metronidazole production method, belonging to the technical field of chemical synthesis. The method sequentially comprises the processes of mixed acid preparation, hydroxylation reaction, formic acid recovery, first neutralization, second neutralization, third neutralization and refining. The process of formic acid recovery specifically comprises the steps of transferring the hydroxylation liquid obtained by the hydroxylation reaction into a distillation kettle, controlling the temperature at 65-90 DEG C and the vacuum degree at (-0.085)-(-0.095)MPa, and performing reduced-pressure distillation to obtain formic acid. According to the metronidazole production method disclosed by the invention, the formic acid is recovered in a metronidazole production process, the usage amount of alkali and the discharge amount of wastewater are reduced, and the production cost is lowered. Meanwhile, the method disclosed by the invention improves the reaction yield of a final product by adjusting the reaction process and parameters.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, in particular to a method for producing metronidazole. Background technique [0002] Metronidazole is also known as metronidazole, metronidazole, metronidazole, metronidazole, etc., and its chemical name is 2-methyl-5-nitroimidazole-1-ethanol (2-methyl-5- nitroimidazole-1-ethanol), is a nitroimidazole synthetic antibacterial drug. It is widely used in clinical practice and has broad-spectrum anti-anaerobic and antiprotozoal effects. It is mainly used in the prevention and treatment of infections caused by anaerobic bacteria, such as respiratory tract, digestive tract, abdominal cavity and pelvic infection, skin soft tissue, bone and bone joints and other parts. infection and endocarditis, brain abscess, sepsis and meningitis caused by Bacteroides fragilis, and is also widely used in the prevention and treatment of oral anaerobic infection. The nitro group of metronidazole is reduced ...

Claims

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Application Information

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IPC IPC(8): C07D233/94
CPCC07D233/94
Inventor 方耀徐双喜段小六周拥军喻莎莎丁文波晏浩哲肖卫国
Owner HUBEI HONGYUAN PHARMA
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