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A kind of synthetic method of tosufloxacin tosylate cyclic compound

A technology of tosufloxacin tosylate and its synthesis method, which is applied in the field of organic compound synthesis, and can solve problems such as difficult recovery, complicated recovery method of dimethylformamide, and non-recyclable solvent.

Active Publication Date: 2021-05-28
赤峰万泽药业股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The recovery method of dimethylformamide is relatively complicated, and it cannot be recovered and stored from water by simple methods such as not adding substances
In the process of synthesizing the target product, N, N-dimethylformamide is required as a reaction solvent. After the synthesis reaction is completed, a large amount of water needs to be added to precipitate the target product, because of the hydrophilicity of N, N-dimethylformamide, and water After mixing, it is difficult to recover high-purity N,N-dimethylformamide through a simple method, which leads to the inability to recycle the solvent and generate a large amount of waste liquid

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Tosufloxacin tosylate cyclic compound of this embodiment is 1-(2,4-difluorophenyl)-6-fluoro-7-chloro-4-oxo-1,4-dihydro-1, The synthetic process of 8-naphthyridine-3-carboxylic acid ethyl ester is:

[0024] First add 500g of dichloromethane (DCM) into the three-necked flask, add 200g of amino under stirring, heat up to 35°C until completely dissolved, add 80g of sodium bicarbonate, and continue the reaction at 35°C for 3 hours. After the reaction is complete, distill Remove dichloromethane, add methanol 300g while hot, stir and disperse for 1 hour, cool down to 5°C, filter and dry the target product at 60°C for 6 hours to obtain 160g of the target product with a yield of 87.6%.

Embodiment 2

[0026] The features of this embodiment that are the same as those of Embodiment 1 will not be described in detail. The features of this embodiment that are different from Embodiment 1 are:

[0027] Tosufloxacin tosylate cyclic compound of this embodiment is 1-(2,4-difluorophenyl)-6-fluoro-7-chloro-4-oxo-1,4-dihydro-1, The synthetic process of 8-naphthyridine-3-carboxylic acid ethyl ester is:

[0028] First add 2000g of dichloromethane into the three-necked flask, add 200g of amino under stirring, heat up to 40°C until completely dissolved, add 200g of sodium bicarbonate, and continue the reaction at 40°C for 3 hours. After the reaction is complete, distill out the dichloromethane Methane, add methanol 300g while hot, stir and disperse for 1 hour, cool down to 8°C, filter and dry the target product at 70°C for 6 hours.

Embodiment 3

[0030] The features of this embodiment that are the same as those of Embodiment 1 will not be described in detail. The features of this embodiment that are different from Embodiment 1 are:

[0031] Tosufloxacin tosylate cyclic compound of this embodiment is 1-(2,4-difluorophenyl)-6-fluoro-7-chloro-4-oxo-1,4-dihydro-1, The synthetic process of 8-naphthyridine-3-carboxylic acid ethyl ester is:

[0032] First add 1000g of dichloromethane into the three-necked flask, add 200g of amino under stirring, heat up to 38°C until completely dissolved, add 160g of sodium bicarbonate, and continue the reaction at 38°C for 3 hours. After the reaction is complete, distill out the dichloromethane Methane, add methanol 300g while hot, stir and disperse for 1 hour, cool down to 7°C, filter and dry the target product at 65°C for 6 hours.

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PUM

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Abstract

The invention discloses a synthesis method of tosufloxacin cyclic compound of toluenesulfonate, which belongs to the technical field of organic compound synthesis. The target compound is synthesized by dissolving an amino compound and an acid salt in a reaction solvent; after the synthesis reaction is completed, the reaction is distilled and recovered Solvent; Wherein, reaction solvent is chlorinated alkanes. In the synthesis method of the present invention, the reaction solvent is replaced by a chlorinated alkane organic solvent, which has a low boiling point and low hydrophilicity, and can be recovered by distillation; dichloromethane with a purity of 99.5% can be obtained Dichloromethane, the yield of dichloromethane reaches more than 85%. When separating the target product, add methanol to disperse the target product. Methanol can effectively dissolve the impurities of the target product and purify the target product during dispersion.

Description

technical field [0001] The present invention relates to the technical field of organic compound synthesis, in particular to a tosufloxacin tosylate cyclic compound (i.e. 1-(2,4-difluorophenyl)-6-fluoro-7-chloro-4-oxo- 1,4-dihydro-1,8-naphthyridine-3-carboxylic acid ethyl ester) synthetic method. Background technique [0002] The carcinogens in the used organic solvents, whether they are volatilized indoors or outdoors, will cause harm to humans, animals and plants. Under the action of sunlight, the solvent gas volatilized into the atmosphere will react in the troposphere of the atmosphere (from the ground to a height of 10km) to generate acid smog, photochemical smog, etc.; organic waste liquid will also escape to the atmospheric stratosphere (the top of the troposphere) to 50km altitude), react with ozone under the action of sunlight, reduce the concentration of ozone, reduce the effect of the ozone layer on absorbing solar ultraviolet rays, thereby reducing the shielding ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D471/04C07C309/30C07C303/32
CPCC07D471/04
Inventor 臧晓明赵凯滕英镡
Owner 赤峰万泽药业股份有限公司