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Environment-friendly method for metronidazole synthesis

A synthesis method and technology of metronidazole are applied in the field of green environmental protection of metronidazole synthesis, which can solve the problems of low profit in metronidazole production and difficulty in separation and removal, and achieve the corrosiveness of green environmental protection equipment, reduce environmental protection pressure, and save energy. resource effect

Active Publication Date: 2016-02-24
WUHAN WUYAO PHARMA
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The invention aims at the problem that the profit of traditional metronidazole production is small, and the generated sewage is difficult to deal with because it contains various organic substances and inorganic salts that are difficult to separate and remove, and provides a green and environmentally friendly method for synthesizing metronidazole and co-producing nitrates

Method used

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  • Environment-friendly method for metronidazole synthesis
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  • Environment-friendly method for metronidazole synthesis

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Effect test

Embodiment 2～5

[0042] Embodiment 2~5 reaction

[0043] Operation process is identical with embodiment 1, and the reaction solution after reaction is respectively marked as reaction solution 2 # ~ Reaction Solution 5 # , the difference is the ratio of raw materials and reaction conditions, as shown in Table 1.

[0044] Table 1 Reaction raw materials and conditions

[0045]

[0046]

Embodiment 6

[0047] Embodiment 6 Separation

Embodiment 1

[0048] After the completion of the reaction in Example 1, the obtained reaction solution 1 # Cool to 50°C, add 200g of methanol, reflux at 60°C for 1 hour, and recover 353g of methyl acetate (purity: 92.1%) by distillation. Add 30% industrial liquid caustic soda at 30°C to adjust the pH to about 2.5, and precipitate nitrate crystals. It was filtered and dried to obtain 304 g of nitrated compounds recovered once. The temperature of the filtrate was controlled at 50° C., and the pH was adjusted to 11 with liquid caustic soda. The crude metronidazole was precipitated, filtered, and dried to obtain 315 g of the crude metronidazole (content 99.1%, melting point 157.6˜159.2° C.). The pH of the filtrate was further adjusted to 5-7 at 40°C, and 20 g of nitrated compounds were precipitated for secondary recovery. The filtrate was concentrated under reduced pressure to about 1 / 4 of the original volume, crystallized at 35° C., filtered, and dried to obtain 476 g of anhydrous sodium sul...

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Abstract

The invention discloses an environment-friendly method for metronidazole synthesis. Formic acid is replaced with acetic acid, alcohol is added for esterification, neutralization is performed for three times, sodium sulfate and ethylene glycol are recovered, a nitration product is effectively recovered from a metronidazole mother solution, derivatives such as acetic ester, anhydrous sodium sulfate and the like are obtained, by-products such as ethylene glycol and the like are chemical raw materials with wide applications, resources are recycled, the raw materials are greatly saved, the production cost is reduced, and the whole novel process adopts simple steps and is convenient to operate.

Description

technical field [0001] The invention belongs to the field of pharmacy, and in particular relates to a green and environment-friendly method for synthesizing metronidazole. Background technique [0002] Metronidazole, chemically named 1-(2-hydroxyethyl)-2-methyl-5-nitroimidazole, is a nitroimidazole antibiotic originally used to treat vaginal trichomoniasis or to kill Anaerobic bacteria that cause oral infection were identified by the World Health Organization as a specific drug against anaerobic infection in 1978, and are widely used in the prevention and treatment of oral anaerobic infection. Metronidazole is also commonly used to prevent and treat respiratory tract, digestive tract, abdominal cavity, pelvic cavity and other infections caused by anaerobic bacteria, skin soft tissue and bone joint infection, pericarditis, sepsis and other diseases. [0003] In the traditional process, metronidazole raw materials use a large amount of raw materials such as formic acid and su...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D233/94
CPCC07D233/94
Inventor 皮金红赵涛涛杨诗宏董建强饶坤仑李彬彬邓军张琦
Owner WUHAN WUYAO PHARMA
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