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Method for synthesizing sulphaguanidine

A synthetic method, the technology of sulfamidine, applied in the preparation of sulfonamide, chemical instruments and methods, and the preparation of organic compounds, etc., can solve the problems of low product yield, high impurity content, difficult to complete reaction between sulfonamide and guanidine nitrate, etc. , to achieve the effect of reducing production complexity, reducing process flow, and controlling product quality

Active Publication Date: 2016-05-25
HUNAN XIANGYIKANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The industrial synthesis method of sulfamidine is to be melted in soda ash by sulfonamide and guanidine nitrate, and the decompression is combined to make, and the applicant finds in production, utilizes disclosed technology to have such defect: (1) the reaction of sulfonamide and guanidine nitrate is difficult Completely, resulting in low product yield
(2) The impurity content of the finished product of the original process is relatively high, especially the endotoxin content is relatively high
However, this method has long reaction steps, high production cost, and high equipment requirements for melting reaction.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Weigh 17.2 g of p-aminobenzene sulfonamide, 9.5 g of guanidine hydrochloride, and 0.086 g of potassium iodide, add 100 ml of water, start stirring and raise the temperature to about 55° C., keep the temperature for 2 hours. Concentrate under reduced pressure to 30% of the original volume, leave to cool, filter, wash the solid with cold water several times, and dry to obtain 20.6 g of crude sulfamidine, with a yield of 96.3%.

[0022] Mix the crude sulfamidine with water, add an appropriate amount of activated carbon, heat to dissolve it, keep it warm and stir for about 0.5h, filter it while it is hot, let it cool to crystallize, filter, rinse the crystals with cold water several times, and dry to obtain pure sulfamidine 18.7g The yield is 90.7% and the purity is 99.5%.

Embodiment 2

[0024] Weigh 17.2 kg of p-aminobenzene sulfonamide, 12.35 kg of guanidine hydrochloride, and 90 g of potassium iodide, add 80 L of water, start stirring and raise the temperature to about 65° C., and react at this temperature for 3 hours. Concentrate under reduced pressure to 30% of the original volume, let cool, filter, wash the solid with cold water several times, and dry to obtain 20.3 kg of crude sulfamidine, with a yield of 94.5%.

[0025] Mix the crude sulfamidine with water, add appropriate amount of activated carbon, heat to dissolve, keep warm and stir for about 0.5h, filter while hot, let cool to crystallize, filter, rinse the crystals with cold water several times, and dry to obtain pure sulfamidine 19.1kg The yield is 94.1%, and the purity is 99.7%.

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Abstract

The invention discloses a method for synthesizing sulphaguanidine. According to the method, sulfonamide and guanidine hydrochloride are used as raw materials and are catalyzed by iodide to synthesize sulphaguanidine in one step. The method has the advantages of short process route and little environment pollution.

Description

Technical field [0001] The invention relates to a method for synthesizing sulfamidine, which belongs to the field of organic synthesis, in particular to the synthesis of sulfamidine raw materials, and also belongs to the technical field of pharmacy. Background technique [0002] Sulfaguanidine (Sulfaguanidine) is a white needle-like crystalline powder. Odorless and tasteless, the color gradually darkens when exposed to sunlight. The melting point is 190~193℃. Slightly soluble in water, ethanol, acetone, soluble in dilute mineral acid and boiling water, insoluble in cold sodium hydroxide solution, can treat various bacillary dysentery, enteritis, and can also be used to prevent bacterial infections before intestinal surgery. The structural formula of sulfamidine is as follows: [0003] . [0004] The industrial synthesis method of sulfamidine is prepared by melting sulfonamide and guanidine nitrate in soda ash and reducing compression. The applicant found in the production that t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C303/40C07C311/64C07C303/36C07C303/44
CPCC07C303/36C07C303/40C07C303/44C07C311/64
Inventor 帅放文王向峰章家伟
Owner HUNAN XIANGYIKANG PHARMA
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