Technology for producing nifuratel

A production process, the technology of nifuratel, applied in the field of production process of nifuratel, can solve the problems of dimethyl sulfate toxicity, complex process, high cost, etc., and achieve the advantages of convenient industrial production, good yield and low cost Effect

Inactive Publication Date: 2016-06-22
ANHUI YOUCARE KAIYUE PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] It can be seen from the analysis of this route that the route uses thiourea and dimethyl sulfate as raw materials, and the process is more complicated and the cost is higher. At the same time, the raw material dimethyl sulfate has great toxicity

Method used

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  • Technology for producing nifuratel
  • Technology for producing nifuratel
  • Technology for producing nifuratel

Examples

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Embodiment Construction

[0030] 1. Production raw materials and dosage

[0031]

[0032]

[0033] 2. Production process

[0034] (1) Synthesis of methylthiopropylene oxide

[0035] Into a 50L reactor, add 7.0kg of epichlorohydrin and 0.5kg of tetrabutylammonium bromide into 15L of dichloromethane in sequence, and after adjusting the temperature to 0±5°C, add 24.8kg of mass fraction into the reaction solution dropwise It is 21.5% sodium methyl mercaptide aqueous solution, the dropping time is controlled at 1.5±0.5 hours, and the temperature is raised to 25±2°C for another 1.5 hours;

[0036] Post-treatment method: stand still to separate the liquid, extract twice with 3.5L dichloromethane, combine the organic phases, wash three times with 10L purified water, remove the dichloromethane at a temperature of 40±5°C under normal pressure, and collect by distillation under reduced pressure Distillation at 45-64°C yielded 4.3 kg of a colorless and odorous liquid (methylthiopropylene oxide), with a mas...

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Abstract

The invention relates to a production process of nifuratel, which comprises the following steps: dissolving epichlorohydrin in dichloromethane, adding tetrabutylammonium bromide, adding sodium methyl mercaptide aqueous solution dropwise, extracting, depressurizing Distillation to obtain methylthio propylene oxide; add methylthio propylene oxide dropwise to hydrazine hydrate under heating conditions, and obtain 3-methylthio-2-hydroxypropyl hydrazine through vacuum distillation; 3-methylthio Base-2-hydroxypropylhydrazine is mixed with diethyl carbonate, sodium methoxide absolute ethanol solution is added, after a ring closure reaction occurs under reflux conditions, vacuum distillation is added, and absolute ethanol is added to obtain (3-amino-5-( Methylthiomethyl)-2-oxazolidinone) absolute ethanol solution, then dropwise added to 5-nitrofurfural, stirred and reacted, filtered, washed with methanol, and dried to obtain the crude product of nifuratel; refined and dried to obtain Nifuratel. The invention has easy-to-obtain raw materials, low cost, good yield, mild reaction conditions, easy mastery and convenient industrial production.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a production process of nifuratel. Background technique [0002] Nifuratel, its chemical name is: 5-[(methylthio)methyl]-3-[[(5-nitro-2-furan)methylene]amino]-2-oxazole Alkanone, the molecular formula is C10H11N3O5S, the chemical structure formula is as follows: [0003] [0004] Nifuratel is a nitrofuran antibiotic drug, which has a significant effect on the treatment of mixed vaginal infections. Its trichomonadicidal activity is equivalent to that of metronidazole, has antibacterial effect, and can effectively kill Chlamydia trachomatis and Mycoplasma, and has certain activity against Candida. Oral and vaginal administration of nifuratel shows that it is well tolerated and has no drug resistance. The cure rate for bacterial vaginosis is equivalent to that of ampicillin and carbenicillin, and the incidence of adverse reactions is significantly lower than that o...

Claims

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Application Information

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IPC IPC(8): C07D413/12
CPCC07D413/12
Inventor 周如国刘维坦高彬洁
Owner ANHUI YOUCARE KAIYUE PHARMA
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