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Method for preparing sulfadimidine salt

A technology of sulfamethazine salt and sulfamethazine, applied in the direction of organic chemistry, etc., to achieve the effect of reducing the possibility of headache

Inactive Publication Date: 2016-08-24
BEIJING HAIJIXING MEDICAL SCI & TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Sulfamethazine is almost insoluble in water. When used, it needs to use organic solvents such as ethanol. The toxicity of ethanol is slightly toxic and can cause headaches and other adverse symptoms.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] A preparation method of sulfamethazine salt, the steps comprising:

[0015] 1) Dissolving step: add sulfuric acid mixed solution into the dissolving tank at 25±5°C, then add 1 weight part of sulfamethazine, 0.01 weight part of sodium bisulfite and 0.1 volume part of aqueous solution, stir for 20 minutes, filter, Obtain solution A; the preparation method of described sulfuric acid mixed solution is, add a kind of solvent in ethanol, methyl alcohol or Virahol in dissolving tank, stir, drip sulfuric acid at 40 ℃, ethanol / methanol / isopropanol: sulfadiene Methazine=4.0~8.0:1, sulfuric acid:sulfamethazine=0.25:1;

[0016] 2) Crystallization step: put solution A in a crystallization tank, stir and crystallize at 35±5°C, cool down to 0°C, and continue stirring for 2 hours to obtain mixed solution B;

[0017] 3) Washing step: filter the mixed solution B, wash the filter cake with a solvent in ethanol, methanol or isopropanol, and take the filter cake C;

[0018] 4) Drying step...

Embodiment 2

[0020] A preparation method of sulfamethazine salt, the steps comprising:

[0021] 1) Dissolving step: add sulfuric acid mixed solution into the dissolving tank at 25±5°C, then add 1 weight part of sulfamethazine, 0.02 weight part of sodium bisulfite and 0.2 volume part of aqueous solution, stir for 30 minutes, filter, Obtain solution A; the preparation method of described sulfuric acid mixed solution is, add a kind of solvent in ethanol, methyl alcohol or Virahol in dissolving tank, stir, drip sulfuric acid at 40 ℃, ethanol / methanol / isopropanol: sulfadiene Methazine=8.0:1, sulfuric acid: sulfamethazine=0.40:1;

[0022] 2) Crystallization step: put solution A in a crystallization tank, stir and crystallize at 35±5°C, cool down to 10°C, and continue stirring for 2 hours to obtain mixed solution B;

[0023] 3) Washing step: filter the mixed solution B, wash the filter cake with a solvent in ethanol, methanol or isopropanol, and take the filter cake C;

[0024] 4) Drying step: ...

Embodiment 3

[0026] A preparation method of sulfamethazine salt, the steps comprising:

[0027] 1) Dissolving step: add sulfuric acid mixed solution into the dissolving tank at 25±5°C, then add 1 weight part of sulfamethazine, 0.013 weight part of sodium bisulfite and 0.13 volume part of aqueous solution, stir for 22 minutes, filter, Obtain solution A; the preparation method of described sulfuric acid mixed solution is, add a kind of solvent in ethanol, methyl alcohol or Virahol in dissolving tank, stir, drip sulfuric acid at 40 ℃, ethanol / methanol / isopropanol: sulfadiene Methazine=5.0:1, sulfuric acid: sulfamethazine=0.27:1;

[0028] 2) Crystallization step: put solution A in a crystallization tank, stir and crystallize at 35±5°C, cool down to 2°C, and continue to stir for 2 hours to obtain mixed solution B;

[0029] 3) Washing step: filter the mixed solution B, wash the filter cake with a solvent in ethanol, methanol or isopropanol, and take the filter cake C;

[0030] 4) Drying step: ...

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PUM

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Abstract

The invention discloses a method for preparing a sulfadimidine salt. The method comprises the following steps: dissolving, washing, crystallizing and drying. According to the method, water serves as a solvent, the toxicity of water is nearly zero, and the headache possibility of a patient is reduced.

Description

technical field [0001] The invention relates to a preparation method of a medical preparation containing a p-benzenesulfonyl N group-containing compound containing one heterocycle, in particular to a preparation method of sulfamethazine salt. Background technique [0002] Sulfamethazine, the Chinese name is N-(4,6-dimethyl-2-pyrimidinyl)-4-aminobenzenesulfonamide, the English name is Sulfamethazinum, and the English abbreviation is SM2. It is a white or slightly yellow crystal or Powder, odorless, slightly bitter taste, dark color gradient when exposed to light, soluble in hot ethanol, insoluble in water or ether, easily soluble in alkenoic acid or dilute alkali solution, is a sulfonamide antibacterial drug, suitable for the treatment of hemolytic For streptococcus, meningococcus, pneumococcus and other infectious diseases, the drug has long-lasting effect, strong antibacterial property, low toxicity and complete absorption speed. [0003] Sulfamethazine is almost insoluble...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D239/69
Inventor 杨军
Owner BEIJING HAIJIXING MEDICAL SCI & TECH CO LTD
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