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Preparation method of sulfanilamide

A technology of aminobenzenesulfonamide and sodium aminobenzenesulfonamide, which is applied in the field of preparation of p-aminobenzenesulfonamide, can solve the problems of inapplicability to industrialization and low yield, and achieve the effect of increasing product yield and reducing total volume

Active Publication Date: 2014-01-01
NANTONG BAISHENG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process is a semi-micro-optimized synthesis process, which is suitable for the basic operation experiments in the basic organic chemistry experiments of school students, and the yield is too low to be suitable for industrialization.

Method used

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  • Preparation method of sulfanilamide

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Effect test

Embodiment 1

[0018] In a 1000ml four-neck flask, add 183g of 20% ammonia water, add 75g of p-acetamidobenzenesulfonyl chloride in batches under stirring, react at 50°C for 2 hours, add 225g of 30% liquid caustic soda, react at 90°C for 2 hours, and use 30% hydrochloric acid Neutralize to a pH value of 6.5, then heat and concentrate, allowing the total volume of the material to be 800ml to concentrate to 600ml, cool to 20°C, filter, and dry to obtain 50g of the product with a yield of 90.12% and a purity of 99.53%.

Embodiment 2

[0020] In a 1000ml four-necked flask, add 225g of 20% ammonia water, add 75g of p-acetamidobenzenesulfonyl chloride in batches under stirring, react at 55°C for 2 hours, add 300g of 30% liquid caustic soda, react at 90°C for 2 hours, and use 30% hydrochloric acid Neutralize to a pH value of 6.8, then heat and concentrate, allowing the total volume of the material to concentrate from 930ml to 700ml, cool to 20°C, filter, and dry to obtain 51.5g of the product with a yield of 92.83% and a purity of 99.52%.

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Abstract

The invention discloses a preparation method of sulfanilamide. The preparation method comprises the steps: adding n-acetylsulfanilyl chloride into ammonium hydroxide, reacting to obtain p-acetamidobenzene sulfamide, adding p-acetamidobenzene sulfamide into sodium hydroxide, hydrolyzing under the alkaline condition to obtain sodium sulfanilamide, reacting the sodium sulfanilamide with hydrochloric acid, directly concentrating under the non-separation condition to obtain the sulfanilamide. The purity of the finished sulfanilamide product obtained by adopting the preparation method can achieve more than 99.5% without the need of recrystallization; the product yield is high and can achieve more than 90%.

Description

technical field [0001] The invention relates to a preparation method of p-aminobenzenesulfonamide. Background technique [0002] P-aminobenzenesulfonamide, referred to as sulfanilamide. Sulfonamides are one of four classes of anti-infective drugs. Due to the good antibacterial effect of sulfonamides, mature technology, easy access to raw materials and low price, after decades of clinical use, they still maintain a certain share. my country is a big producer of sulfonamides and a big user of the drug, with an annual output of about 10,000 tons. Most of them are sold to overseas markets. Using acetanilide as a raw material, prepare p-acetamidobenzenesulfonyl chloride by chlorosulfonation with chlorosulfonic acid, then undergo ammonolysis to obtain acetamidobenzenesulfonamide, and undergo hydrolysis and recrystallization to obtain the final product sulfonamide. [0003] Data report takes acetanilide as the technique for raw material preparation of sulfonamide as follows: ...

Claims

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Application Information

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IPC IPC(8): C07C311/39C07C311/46C07C303/36
Inventor 张天永邓永锋袁仲飞
Owner NANTONG BAISHENG CHEM
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