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Synthesis method of furazolidone

A synthetic method, the technology of furazolidone, applied in the field of organic chemical synthesis, can solve the problems of complex equipment and low yield, and achieve the effects of simple equipment, high product yield and reduced risk

Active Publication Date: 2013-04-24
衢州伟荣药化股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process uses a distillation tower with complex equipment; methanol and ethanol are used as solvents for the final condensation; the yield is low; therefore, it has not been used in industrial production

Method used

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  • Synthesis method of furazolidone
  • Synthesis method of furazolidone
  • Synthesis method of furazolidone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] First add 250g of 80% hydrazine hydrate, raise the temperature to 70°C, and start to vaporize ethylene oxide. The ethylene oxide gas passes through a 5-meter coil, and the coil is placed in 70°C water, and the hot ethylene oxide gas is passed into In hydrazine hydrate, control the aeration speed, the temperature of hydrazine hydrate is 70°C, the time of aeration of 23.7g is about 1.5 hours, and the temperature is kept at 70°C for 1 hour. Then, 60g of hydrazine hydrate was distilled off at atmospheric pressure (the content is more than 50%, and the hydrazine hydrate content was more than 70% after steaming part of the water), and then the hydrazine hydrate was collected by vacuum distillation (the content was above 70°C, the hydrazine hydrate was always Apply mechanically), until the temperature reaches 135°C, evaporate the hydrazine hydrate to dryness as much as possible. 40 g of β-hydroxyethylhydrazine was obtained.

[0039]Cool 40g of β-hydroxyethylhydrazine to 50°C,...

Embodiment 2

[0043] First add 250g of 80% hydrazine hydrate, raise the temperature to 65°C, and start to vaporize ethylene oxide. The ethylene oxide gas passes through a 3-meter coil, and the coil is placed in 50°C water, and the hot ethylene oxide is passed through to hydrate In hydrazine, control the aeration rate, the temperature of hydrazine hydrate is 65°C, the time of aeration of 23.7g is about 1.5 hours, and the temperature is kept at 65°C for 1 hour. Then, 60g of hydrazine hydrate was distilled off at atmospheric pressure (the content is more than 50%, and the hydrazine hydrate content was more than 70% after steaming part of the water), and then the hydrazine hydrate was collected by vacuum distillation (the content was above 70°C, the hydrazine hydrate was always Applicable), until the temperature reaches 140°C, evaporate the hydrazine hydrate to dryness as much as possible. 40 g of β-hydroxyethylhydrazine was obtained.

[0044] Cool 40g of β-hydroxyethylhydrazine to 50°C, first...

Embodiment 3

[0048] First add 285.7g of 70% recovered hydrazine hydrate, and start to vaporize ethylene oxide. The ethylene oxide gas passes through a 100-meter coiled pipe, and the coiled pipe is placed in 70°C water, and the hot ethylene oxide is passed into the hydrazine hydrate. Control the aeration speed, the temperature of hydrazine hydrate is at 70°C, the aeration time of 23.7g is about 1.5 hours, and the temperature is kept at 70°C for 1 hour. Then, 60g of hydrazine hydrate was distilled off at atmospheric pressure (the content is more than 50%, and the hydrazine hydrate content was more than 70% after steaming part of the water), and then the hydrazine hydrate was collected by vacuum distillation (the content was above 70°C, the hydrazine hydrate was always Applicable), until the temperature reaches 130°C, evaporate the hydrazine hydrate to dryness as much as possible. 40 g of β-hydroxyethylhydrazine was obtained.

[0049] Cool 40g of β-hydroxyethylhydrazine to 50°C, first add 8....

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Abstract

The invention belongs to the field of organic chemical synthesis, and particularly relates to a synthesis method of furazolidone. The synthesis method comprises the following steps: introducing gasified ethylene oxide into a hydrazine hydrate through a coiler placed in hot water so as to prepare beta-hydroxyethylhydrazine; after cooling the beta-hydroxyethylhydrazine, adding sodium methoxide methyl alcohol solution and then stirring, and adding dimethyl carbonate so as to prepare 3-amino-2-oxazolidinone; and adding water in 3-amino-2-oxazolidinone, adding hydrochloric acid, rising the temperature, adding 5-nitryl furfural ester diacetate, and carrying out periodical warming so as to obtain the finished furazolidone. By using the synthesis method, the problems that the process is not environment-friendly, the requirement on equipment is high, the yield of the product is low, and the like in the prior art are effectively solved, and the yield of the product in the invention can be improved by 5-10%.

Description

technical field [0001] The invention belongs to the field of organic chemical synthesis, and specifically relates to a synthesis method of furazolidone with simple process conditions, easy to be used in large-scale production, energy saving and environmental protection, and low production cost. Background technique [0002] Furazolidone, chemical name: "3-(5-nitrofurylmethylidene)-2-oxazolidinone", has a broad antibacterial spectrum, and the most sensitive bacteria are Escherichia coli, Bacillus anthracis, Bacillus paratyphi, and Shigella wait. The present stage mainly contains about the synthetic technique of furazolidone: [0003] Process route 1 (used in industrial production): heating and condensation of ethanolamine and urea, nitrosation, cyclization, re-nitrosation, and reduction to obtain 3-amino-2-oxazolidinone; then combined with 5-nitrofurfural Condensation gives furazolidone. This process is not environmentally friendly, has a lot of waste gas and waste water, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D413/12
Inventor 曹桂东吴伟荣曹桂平
Owner 衢州伟荣药化股份有限公司
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