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Preparation method of norfloxacin and refining process thereof

The technology of norfloxacin and process is applied in the field of preparation of norfloxacin, which can solve the problems of high cost, cumbersome steps and high reaction temperature, and achieve the effects of less by-products, low reaction temperature and improved yield.

Inactive Publication Date: 2018-07-13
SHANXI YUNPENG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The present synthetic method of norfloxacin is costly, and the steps are loaded down with trivial details, and reaction temperature is high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] A preparation method of norfloxacin, comprising the following steps:

[0034] S1. Add 25g (0.11mol) of 2,4-dichloro-5-fluorobenzoyl chloride and an acid-binding agent into the reaction kettle, and add 9.45g (0.066mol) of ethyl N,N-dimethylaminoacrylate under stirring, Control the temperature of the reaction solution to 70°C, and keep stirring for 3 hours;

[0035] S2. Add 40.66g (0.44mol) toluene and 3.96g (0.22mol) water to the S1 reaction solution, add hydrochloric acid to adjust the pH to 1-2, stir evenly, let stand to separate layers, separate the organic layer, wash with water until medium property, distill off the remaining moisture, and transfer the organic phase to the autoclave;

[0036] S3. Lower the temperature of the organic phase in S2 to 15°C, add 0.99g (0.022mol) ethylamine dropwise, and introduce CO 2 Gas, control the reaction pressure to be 2atm, after reacting for 3h, recover N by distillation, and the N-dimethylamine complex, the mother liquor is fo...

Embodiment 2

[0052] S1. Add 25g (0.11mol) of 2,4-dichloro-5-fluorobenzoyl chloride and an acid-binding agent into the reaction kettle, and add 11.025g (0.0725mol) of N,N-dimethylaminoacrylate under stirring, Control the temperature of the reaction solution to 70°C, and keep stirring for 3 hours;

[0053] S2. Add 50.82g (0.55mol) of toluene and 5.94g (0.33mol) of water to the S1 reaction solution, add hydrochloric acid to adjust the pH to 1-2, stir evenly, let it stand for stratification, separate the organic layer, wash it with water until medium property, distill off the remaining moisture, and transfer the organic phase to the autoclave;

[0054] S3. Lower the temperature of the organic phase in S2 to 15°C, add 2.475g (0.055mol) ethylamine dropwise, and introduce CO 2 Gas, the control reaction pressure is 2atm, after reacting for 5h, distillation recovery N, N-dimethylamine complex, the mother liquor is for subsequent use;

[0055] S4. Add 50.82g (0.55mol) toluene and 1.76g (0.044mol) ...

Embodiment 3

[0070] S1. Add 25g (0.11mol) of 2,4-dichloro-5-fluorobenzoyl chloride and an acid-binding agent into the reaction kettle, and add 10.25g (0.072mol) of N,N-dimethylaminoacrylate under stirring, Control the temperature of the reaction solution to 70°C, and keep stirring for 3 hours;

[0071] S2. Add 45.68g (0.49mol) toluene and 4.84g (0.27mol) water to the S1 reaction solution, add hydrochloric acid to adjust the pH to 1-2, stir evenly, let stand to separate layers, separate the organic layer, wash with water until medium property, distill off the remaining moisture, and transfer the organic phase to the autoclave;

[0072] S3, lower the temperature of the organic phase in S2 to 15°C, add 1.56g (0.035mol) ethylamine dropwise, and introduce CO 2 Gas, the control reaction pressure is 2atm, after reacting for 5h, distillation recovery N, N-dimethylamine complex, the mother liquor is for subsequent use;

[0073] S4. Add 45.68g (0.49mol) toluene and 1.57g (0.039mol) sodium hydroxid...

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Abstract

The invention relates to the technical field of pharmaceutical synthesis, and more particularly relates to a preparation method of norfloxacin and a refining process thereof. By adopting triethylamineor K2CO3 acid acceptor, the reaction efficiency is improved; by adopting a Lewis acid, the efficiency is improved, the cost is reduced, the reaction temperature is low and a byproduct is less; meanwhile, great use of an inorganic acid and inorganic base can be avoided, pollution from the three wastes is reduced, and coarse norfloxacin is also refined, so that the high-purity norfloxacin is prepared; therefore, the quality of norfloxacin is further improved, a result product is qualified, a conclusion and process operation is feasible, and the preparation method is suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of drug synthesis, and more specifically, relates to a preparation method of norfloxacin and a refining process thereof. Background technique [0002] Norfloxacin is a third-generation quinolone antibacterial drug, which can hinder the action of DNA gyrase (DNAGyrase) of pathogenic bacteria in the digestive tract, hinder bacterial DNA replication, and have an inhibitory effect on bacteria. It is a commonly used medicine for the treatment of enteritis and dysentery. The present synthetic method of norfloxacin is costly, and the steps are loaded down with trivial details, and reaction temperature is high. Contents of the invention [0003] In order to overcome the deficiencies in the prior art, the invention provides a preparation method of norfloxacin with few steps and low cost and a refining process of norfloxacin to provide high-purity norfloxacin. [0004] In order to solve the problems of the technol...

Claims

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Application Information

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IPC IPC(8): C07D215/56
CPCC07D215/56
Inventor 文献江
Owner SHANXI YUNPENG PHARMA
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