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Method for preparing nifuratel

A technology of nifuratel and a synthesis method, which is applied in the field of drug synthesis, can solve the problems of decreased yield, low yield of nifuratel, difficult control of high vacuum, etc., and achieves low environmental pollution and simple and easy-to-control synthesis method. , the effect of improving yield

Inactive Publication Date: 2013-08-07
NAT INST OF PHARMA R & D CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

On the basis of fully studying the above-mentioned route, it is found that there are following problems in the prior art: 1. in the synthetic step of 3-methylthio-2-hydroxyl-propylhydrazine, the post-processing method of high vacuum vacuum distillation is selected to purify the intermediate 3- Methylthio-2-hydroxyl-propylhydrazine, although the intermediate purity obtained by the post-treatment method is high, the yield decreases, and high vacuum is difficult to control in industrial production; 2. the yield of nifuratel is not high ;

Method used

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  • Method for preparing nifuratel
  • Method for preparing nifuratel
  • Method for preparing nifuratel

Examples

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Embodiment 1

[0037] Pump 18.2 Kg of 80% hydrazine hydrate into a 50L clean reactor, raise the temperature of the reaction solution to 80-85°C, and gradually add 11 kg of methylthiopropylene oxide under mechanical stirring. During the dropwise addition, the reaction is violently exothermic. The reaction temperature should be strictly controlled not to exceed 95°C. After the addition, the reaction was continued for 4 hours at 90-95°C. Control the reaction liquid at 80-85°C to distill hydrazine hydrate under reduced pressure (vacuum degree control ≤0.09MPa), carry out reduced-pressure distillation under this vacuum condition until no liquid is evaporated; then cool the reaction kettle to 60-65°C to remove Pressure device, add 6 kg of absolute ethanol, stir for 20 minutes, then connect the decompression device for distillation, and raise the temperature to 80-85°C (vacuum degree control ≤0.09MPa) until no liquid evaporates; repeat the above operation of 6 kg of absolute ethanol Twice, a total...

Embodiment 2

[0039] Add 7.3 kg of anhydrous methanol into a 25L plastic bucket, add 1.3 kg of sodium methoxide under stirring, and dissolve to obtain a methanol solution of sodium methoxide for use (the reaction liquid has no temperature limit, but anhydrous operation must be ensured); in intermediate A 1 12.4 kg of diethyl carbonate was added to the 50L reaction kettle under stirring, and after stirring for 15 minutes, the prepared sodium methoxide methanol solution was added dropwise to the reaction solution, and the dropwise addition was completed in 0.5 hours, and then the temperature was raised to 60-70°C The reaction was refluxed for 3 hours. Cool the reactor to 20-25°C, then add 8.0 kg of absolute ethanol and stir for 15 minutes to obtain A 2 ethanol solution, set aside.

Embodiment 3

[0041]Pump 47.0 kg of water into a 100L reactor, gradually add 5.5 kg of concentrated sulfuric acid under stirring, and stir the reaction solution evenly to obtain a 10% dilute sulfuric acid solution for subsequent use; pump 44.0 kg of 95% ethanol into a 200L reactor, stir 5-nitrofurfural diethyl ester (B 1 ) 25.0 kg was added to the reaction kettle, and the reaction solution was fully stirred evenly, and then the prepared 10% dilute sulfuric acid solution was gradually added dropwise. The reaction kettle was lowered to room temperature for use.

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Abstract

The invention belongs to the field of drug synthesis and provides a novel method for synthetizing nifuratel. The synthesis method of the nifuratel disclosed by the invention innovatively adopts a post-treatment method of 'ethanol with water' to obtain a midbody 3-methyl mercapto-2-hydroxy propyl hydrazine (A1); high-vacuum reduced pressure distillation of the midbody 3-methyl mercapto-2-hydroxy propyl hydrazine (A1) is avoided; the nifuratel is prepared by a 'one-pot' method; preparation of a midbody N-amino-5-methylthiomethyl-2-oxazolidinone (A2) and post-treatment operation of 5-nitro-furfural (B1) are simplified; the purity of the obtained nifuratel product is higher than 99.8%; and the yield is higher than 30%. The synthesis method of nifuratel disclosed by the invention is simple, convenient and easy to control; the post-treatment operation is simple and feasible; industrialized production is facilitated; the used material is available in China; the pollution on the environment is small; and the material is cheap and easily available.

Description

technical field [0001] The invention belongs to the field of medicine synthesis and relates to a synthesis method of nifuratel. Background technique [0002] Nifutel (Nifutatel) is a nitrofuran derivative, the chemical name is 5-[(methylthio)methyl]-3-[[(5-nitro-2-furan)methylene]amino]-2 - Oxazolidinone is a new drug mainly used for gynecological mixed infection exclusively developed and produced by Italian PoLi Chemical Industry Company. The drug is a broad-spectrum antibiotic, especially has a strong killing effect on common pathogens of gynecological infections such as Gram-positive and negative bacteria, trichomonas, molds, chlamydia and mycoplasma. It has a good curative effect on the treatment of common gynecological vaginal infections caused by trichomonas, Candida albicans, and bacteria. At present, it is listed in my country and many other countries in dosage forms such as tablets and capsules. [0003] By consulting the literature, it is found that in the synth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D413/12
Inventor 张淑兰王毅飞辛丕明宗利斌
Owner NAT INST OF PHARMA R & D CO LTD
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