Method for synthesizing CLT acid

A technology of chlorobenzenesulfonic acid and carbon monoxide, which is applied in the fields of sulfonic acid preparation, chemical recovery, organic chemistry, etc., can solve the problems of serious pollution, complicated operation, and many steps, and achieve high reaction selectivity, simple raw materials, and low cost Effect

Active Publication Date: 2014-03-26
LIAONING UNIVERSITY
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Problems solved by technology

The disadvantage of the above method is that there are many steps, complex operation, low yield and serious pollution

Method used

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  • Method for synthesizing CLT acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Add 2-nitro-4-methyl-5-chlorobenzenesulfonic acid (50mmol), selenium powder (0.3g) into a 1000ml autoclave equipped with a stirring bar, H 2 O (400ml), Na 2 CO 3 (22g), add carbon monoxide to 4MPa, then heat to 130°C, stir and react for 6 hours, after cooling to room temperature, add hydrochloric acid to acidify and precipitate precipitate, vacuum-dry after suction filtration, and the target product can be obtained.

[0019] According to the national standard GB / T23670-2009, the yield of CLT acid was 99.8%.

Embodiment 2

[0021] The reaction temperature was 140° C., and the time was 6 hours. Other experimental methods and conditions were the same as in Example 1, and the measured yield was 90.1%.

Embodiment 3

[0023] The reaction time was 4 hours, and other experimental methods and conditions were the same as in Example 1, and the yield was 98.3%.

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Abstract

The invention relates to a method for synthesizing CLT acid, which has the technical scheme that 2-nitro-4-methyl-5-chlorobenzenesulfonic acid is taken as raw material; under the condition that carbon monoxide and water exist, selenium is taken as catalyst, inorganic base or organic base is taken as catalyst promoter; and reaction is carried out at high temperature and high pressure, so that the CLT acid can be synthesized by a one-step method. The method is simple, convenient and safe, realizes aqueous phase reaction, and is easy in obtaining of raw material, free from pollution, high in selectivity and high in yield; and the catalyst can be recycled after the reaction.

Description

technical field [0001] The present invention relates to the synthesis of CLT acid, in particular to a method for synthesizing CLT with selenium and 2-nitro-4-methyl-5-chlorobenzenesulfonic acid as raw materials in the presence of water and carbon monoxide under high temperature and high pressure sour method. Background technique [0002] CLT acid, the chemical name is 5-amino-2-chlorotoluene-4-sulfonic acid (also known as 6-chloro-3-aminotoluene-4-sulfonic acid), referred to as C acid. It is an important intermediate for the synthesis of red organic pigments. It is mainly used to synthesize golden red C and other pigments in industry, and is also widely used in the coloring of paints, coatings, inks, rubber, and plastic products. At present, conventional methods for synthesizing CLT acid include: synthesis of CLT acid from o-chlorotoluene, liquid-phase catalytic hydrogenation, and phosgene synthesis of toluidine. The disadvantage of the above method is that there are many...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C309/48C07C303/22
CPCY02P20/584
Inventor 刘晓智刘士枕张欣李俊杨龙全凤玲兰诗龙高扬
Owner LIAONING UNIVERSITY
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