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Method for preparing sodium sulfamonomethoxine

A technology of sulfa-metamethoxine and sodium methotrexate, which is applied in the field of veterinary drug preparation, can solve the problems of large amount of alkali waste liquid, low yield, and high impurity content in products, and achieve less alkali waste liquid, high yield, and high product quality. The effect of high purity

Inactive Publication Date: 2019-01-04
ZHENGZHOU HOUYI PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The amount of alkali waste liquid produced by this method is large, the yield is low, and the impurity content of the product is high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] A preparation method of sulfamethoxine sodium, comprising the following steps: (1) adding sulfamethoxine and sodium hydroxide into water, and stirring and reacting for 0.8-1.2 hours at a temperature of 70-90°C;

[0019] (2) Adjust the pH value of the reaction solution to 9.80-10.50, add 0.2-0.4% activated carbon of the mass of sulfamethoxine, stir for 0.3-0.8 hours to decolorize, and filter while it is hot to obtain the filtrate;

[0020] (3) Distill the filtrate under reduced pressure, steam until the water content is less than or equal to 10%, then add alcohol, stir and heat, and reflux for 30-60 minutes;

[0021] (4) Then cool the reaction solution obtained in step (3) at 0-5°C for 3.5-5 hours, and filter;

[0022] (5) washing the filter residue obtained in step (4) with alcohol, and drying in vacuum at 55-60° C. for 2.5-4 hours to obtain sulfamethoxine sodium.

Embodiment 2

[0024] A preparation method of sulfamethoxine sodium, comprising the following steps: (1) adding 100 g of sulfamethoxine and 13 g of sodium hydroxide into 400 ml of water, and stirring and reacting for 1.0 hour at a temperature of 75° C.;

[0025] (2) Add acid or alkali to adjust the pH of the reaction solution to 9.85, add 0.3 g of activated carbon, stir for 30 minutes to decolorize, and filter while it is hot to obtain the filtrate;

[0026] (3) Distill the filtrate under reduced pressure for 3 hours until the water content is 3%, add 200ml of ethanol, stir and heat, and reflux for 45 minutes;

[0027] (4) Then cool the reaction liquid obtained in step (3) at 0°C for 4 hours, and filter;

[0028] (5) Wash the filter residue obtained in step (4) with ethanol, and dry it in vacuum at 58° C. for 3 hours to obtain 20.88 g of sulfamethoxine sodium, with a yield of 96.82% and a purity of 99.92%.

Embodiment 3

[0030] A preparation method of sulfamethoxine sodium, comprising the following steps: (1) adding 100 g of sulfamethoxine and 15 g of sodium hydroxide into 800 ml of water, and stirring and reacting for 0.8 hours at a temperature of 70° C.;

[0031] (2) Add acid or alkali to adjust the pH of the reaction solution to 9.80, add 0.3 g of activated carbon, stir for 30 minutes to decolorize, and filter while it is hot to obtain the filtrate;

[0032] (3) Distill the filtrate under reduced pressure for 2 hours until the water content is 8%, add 250ml of ethanol, stir and heat, and reflux for 30 minutes;

[0033] (4) Then cool the reaction liquid obtained in step (3) at 5°C for 3.5 hours, and filter;

[0034] (5) The filter residue obtained in step (4) was washed with ethanol, and vacuum-dried at 55° C. for 2.5 hours to obtain 21.03 g of sulfamethoxine sodium, with a yield of 97.50% and a purity of 99.25%.

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Abstract

The invention provides a method for preparing sodium sulfamonomethoxine. The method comprises the following steps: (1) putting sulfamonomethoxine and sodium hydroxide into water, and stirring to reactfor 0.8-1.2 hours at 70-90 DEG C; (2) adjusting the pH value of the reaction liquid to 9.80-10.50, adding activated carbon which accounts for 0.2-0.4% of the sulfamonomethoxine, stirring and decoloring for 0.3-0.8 hours, and filtering the hot liquid so as to obtain filtrate; (3) carrying out vacuum distillation on the filtrate till the water content is smaller than or equal to 10%, adding alcohol, stirring, heating, and backflowing for 30-60 minutes; (4) cooling the reaction liquid obtained in the step (3) 3.5-5 hours at 0-5 DEG C, and filtering; (5) washing filtrate residues obtained in thestep (4) with alcohol, and carrying out vacuum drying for 2.5-4 hours at 55-60 DEG C, so as to obtain the sodium sulfamonomethoxine. The method for preparing the sodium sulfamonomethoxine, which is provided by the invention, is small in waste alkali amount in the production process and high in yield, and the prepared product is high in purity.

Description

technical field [0001] The invention relates to the field of veterinary drug preparation, in particular to a preparation method of sulfamethoxine sodium. Background technique [0002] Sulfamethoxine sodium is a long-acting new sulfonamide drug with the strongest antibacterial effect in vivo and in vitro. It has a strong inhibitory effect on most Gram-positive and Gram-negative bacteria, and it is not easy to develop drug resistance. It has a significant curative effect on various diseases caused by sensitive bacteria, Toxoplasma gondii, Eperythrozoon and their mixed infections. [0003] The common method for preparing sulfamethoxine sodium at present is to react sulfamethoxine with sodium hydroxide solution, and the reaction solution is decolorized, filtered, and dried to obtain sulfamethoxine sodium. The amount of alkali waste liquid produced by this method is large, the yield is low, and the impurity content of the product is high. Contents of the invention [0004] In...

Claims

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Application Information

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IPC IPC(8): C07D239/69
CPCC07D239/69
Inventor 李建正李娜
Owner ZHENGZHOU HOUYI PHARMA
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