Preparation method of high-purity sulfanilamide

A high-purity, sulfonamide technology, applied in the preparation of sulfonic acid amide, sulfonic acid, organic compounds, etc., can solve the problem of a large number of by-products, and achieve the effect of less by-products, good material fluidity and uniform reaction system

Inactive Publication Date: 2018-07-06
安徽新世纪药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of this invention is to provide a kind of preparation method of high-purity sulfonamide, sol

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] A preparation method for high-purity sulfonamides, specifically comprising the following steps: 1) Chlorosulfonation reaction: m-chloroaniline, chlorosulfonic acid, and phosphorus trichloride are prepared in a molar ratio of 1:2.8:1, and chlorosulfonic acid is mixed at 1.5 Add dropwise to m-chloroaniline at a temperature of 35°C within 1 hour, and maintain the first mixed solution for 10 minutes after the dropwise addition; then add the phosphorus trichloride dropwise to the first mixed solution at a temperature of 35°C within 1.5 hours. In the liquid, stir while adding it dropwise, and add carbon tetrachloride into the reaction vessel as a protective solvent; then turn on the steam for heating, so that the temperature of the material liquid rises to 90°C, turn off the steam, let it naturally heat up to 100°C, and add Cuprous chloride with 5% m-chloroaniline mass was incubated at 100°C for 1.5 hours;

[0023] 2) Stand still: Step 1) After the heat preservation is over, ...

Embodiment 2

[0029] A preparation method for high-purity sulfonamides, specifically comprising the following steps: 1) Chlorosulfonation reaction: m-chloroaniline, chlorosulfonic acid, and phosphorus trichloride are prepared in a molar ratio of 1:3.0:1.1, and chlorosulfonic acid is mixed in 2 Add dropwise to m-chloroaniline at a temperature of 50°C within hours, and maintain the first mixed solution for 30 minutes after the dropwise addition; then add the phosphorus trichloride dropwise to the first mixed solution at a temperature of 50°C within 2 hours. In the liquid, stir while adding it dropwise, and add carbon tetrachloride into the reaction vessel as a protective solvent; then turn on the steam to heat, so that the temperature of the material liquid rises to 100°C, turn off the steam, let it naturally rise to 110°C, add Cuprous chloride with 15% m-chloroaniline mass was incubated at 110°C for 3.5 hours;

[0030] 2) Stand still: Step 1) After the heat preservation is over, stop stirrin...

Embodiment 3

[0036]A preparation method for high-purity sulfonamides, specifically comprising the following steps: 1) Chlorosulfonation reaction: m-chloroaniline, chlorosulfonic acid, and phosphorus trichloride are prepared in a molar ratio of 1:3.6:1.8, and chlorosulfonic acid is mixed at 1.8 Add dropwise to m-chloroaniline at a temperature of 55°C within hours, and maintain the first mixed solution for 25 minutes after the dropwise addition; then add the phosphorus trichloride dropwise to the first mixed solution at a temperature of 55°C within 2 hours. In the liquid, stir while adding it dropwise, and add carbon tetrachloride into the reaction vessel as a protective solvent; then turn on the steam for heating, so that the temperature of the material liquid rises to 95°C, turn off the steam, let it naturally heat up to 115°C, add The cuprous chloride of m-chloroaniline quality 25%, was incubated at 115 ℃ for 3 hours;

[0037] 2) Stand still: Step 1) After the heat preservation is over, s...

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PUM

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Abstract

The invention discloses a preparation method of high-purity sulfanilamide. The preparation method specifically comprises the following steps that (1) a chlorosulfonation reaction is conducted, specifically, m-chloroaniline, chlorosulfonic acid and phosphorus trichloride are mixed at the molar ratio of 1:(2.8-3.6):(1-1.8), chlorosulfonic acid is added dropwise within 1.5-2 hours in m-chloroanilinewith the temperature being 35-55 DEG C, after dripping is ended, the mixed liquid is maintained for 10-30 minutes, and first mixed liquid is obtained; phosphorus trichloride is added dropwise into thefirst mixed liquid; and heating is conducted to make the temperature of the mixed product rise to 100-115 DEG C, and heat preservation is conducted for 1.5-3.5 hours at the temperature of 100-115 DEGC; (2) standing is conducted; (3) a chlorosulfonated substance is obtained; (4) an ammoniation reaction is conducted; and (5) refining is conducted, specifically, the obtained amide is subjected to dissolution decoloration and crystallization and purification. By controlling the adding sequence, frequency and amount requirements of the reactants, the reaction can be conducted more sufficiently and safer, the generated by-products are less, obtaining of high-purity sulfanilamide can be ensured, and the main component (4-amino-chloro-1,3-benzendisulfonamide) of high-purity sulfanilamide can beas high as 99.9% or above.

Description

technical field [0001] The invention relates to a preparation method of sulfonamide, in particular to a preparation method of high-purity sulfonamide. Background technique [0002] Sulfonamides (SAs) refer to the general term of a class of drugs with the structure of sulfanilamide, and are a class of chemotherapeutic drugs used to prevent and treat bacterial infectious diseases. There are thousands of SAs, among which There are dozens of kinds that are widely used and have certain curative effects. Sulfa drugs are a class of antibacterial and anti-inflammatory drugs commonly used in modern medicine. There are many varieties of them, and they have become a huge "family". [0003] Sulfonamide drugs are generally white or slightly yellow crystalline powder, which is easy to deteriorate when exposed to light, and the color gradually becomes darker. Most of these drugs have extremely low solubility in water and are relatively soluble in dilute alkali, but they are easily soluble ...

Claims

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Application Information

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IPC IPC(8): C07C311/39C07C303/38C07C303/44C07C303/08C07C309/48
CPCC07C303/08C07C303/38C07C303/44C07C309/48C07C311/39
Inventor 冯书影周月韦勇申团结
Owner 安徽新世纪药业有限公司
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