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Synthetic method for organic synthesis intermediate metanilic acid

An aminobenzenesulfonic acid and organic synthesis technology, applied in the preparation of sulfonic acid, organic chemistry, etc., can solve the problems of complex process and low final yield, and achieve the advantages of reducing intermediate links, shortening reaction time, and improving reaction yield. Effect

Inactive Publication Date: 2018-08-14
CHENGDU ZHONGHENG HUATIE TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, most of the existing synthetic methods adopt benzene as the reactant, the process is more complicated, and the final yield is not very high. Therefore, it is necessary to propose a new synthetic method, which will further improve the quality and yield of the product, reduce the By-product content is economically important

Method used

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  • Synthetic method for organic synthesis intermediate metanilic acid

Examples

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Effect test

example 1

[0011] Add 2mol of 3-methylaniline in the reaction vessel, 3mol of mass fraction is 30% sulfuric acid solution, 10g of alumina powder, raise the solution temperature to 40°C, control the stirring speed at 90rpm, after stirring for 90min, raise the solution temperature to 70°C, reflux for 30min, wash with a mass fraction of 15% potassium bromide solution, wash with a mass fraction of 35% cyclohexane solution, wash with a mass fraction of 45% butanone solution, and dehydrate with a phosphorus pentoxide dehydrating agent. Recrystallized in 70% isopropanol solution to obtain 306.24 g of crystalline m-aminobenzenesulfonic acid with a yield of 88%.

example 2

[0013] Add 2mol of 3-methylaniline, 3.5mol of sulfuric acid solution, and 11g of alumina powder into the reaction vessel, raise the solution temperature to 42°C, control the stirring speed to 100rpm, stir for 95min, raise the solution temperature to 75°C, and reflux 35min, mass fraction is 17% potassium bromide solution washing, mass fraction is 37% cyclohexane solution washing, mass fraction is 47% butanone solution washing, anhydrous potassium carbonate dehydrating agent is dehydrated, and mass fraction is 75% isopropyl Recrystallized in alcohol solution to obtain 316.68 g of crystalline m-aminobenzenesulfonic acid with a yield of 91%.

example 3

[0015] In the reaction vessel, add 2mol of 3-methylaniline, 4mol mass fraction of 40% sulfuric acid solution, 13g of aluminum oxide powder, raise the solution temperature to 45°C, control the stirring speed to 110rpm, and after stirring for 110min, raise the solution temperature to 80°C, reflux for 40min, wash with a mass fraction of 20% potassium bromide solution, wash with a mass fraction of 40% cyclohexane solution, wash with a mass fraction of 50% butanone solution, and dehydrate with a phosphorus pentoxide dehydrating agent. Recrystallized in 80% isopropanol solution to obtain 323.64 g of crystalline m-aminobenzenesulfonic acid with a yield of 93%.

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Abstract

The invention relates to a synthetic method for organic synthesis intermediate metanilic acid. The method mainly comprises the following steps: adding 2 mol of 3-methylaniline, 3-4 mol of a sulfuric acid solution and 10-13 g of aluminum oxide powder into a reaction vessel, raising the solution temperature to 40-45 DEG C, controlling a stirring speed to be 90-110 rpm, performing stirring for 90-110min, raising the solution temperature to 70-80 DEG C, performing reflux for 30-40 min, performing washing by using a potassium bromide solution, performing washing by using a cyclohexane solution, performing washing by using a butanone solution, performing dehydration by using a dehydrating agent, and performing recrystallization in an isopropanol solution to obtain the crystal metanilic acid.

Description

technical field [0001] The invention relates to a method for synthesizing an organic synthesis intermediate m-aminobenzenesulfonic acid. Background technique [0002] M-aminobenzenesulfonic acid is mainly used in the production of anticancer drugs, pesticides, imaging agents, etc. However, most of the existing synthetic methods adopt benzene as the reactant, the process is more complicated, and the final yield is not very high. Therefore, it is necessary to propose a new synthetic method, which will further improve the quality and yield of the product, reduce the The by-product content is of great economic importance. Contents of the invention [0003] The object of the present invention is to provide a kind of synthetic method of organic synthesis intermediate m-aminobenzenesulfonic acid, comprising the steps: [0004] (i) Add 2mol of 3-methylaniline, 3-4mol of sulfuric acid solution, 10-13g of alumina powder into the reaction vessel, increase the temperature of the sol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C303/06C07C309/46
CPCC07C303/06C07C309/46
Inventor 彭响亮
Owner CHENGDU ZHONGHENG HUATIE TECH CO LTD