Method for synthesizing M acid

A technology of carbon monoxide and trimethylbenzenesulfonic acid, which is applied in chemical instruments and methods, sulfonic acid preparation, organic chemistry, etc., can solve the problems of easy deactivation of catalysts, influence of reaction process, increase of catalyst cost investment, etc., to avoid The effect of high three wastes, simple operation, easy separation, recycling and reuse

Inactive Publication Date: 2019-11-12
LIAONING UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But because there is a small amount of sulfur in the M acid nitro, the catalyst is easily deactivated during the catalytic hydrogenation process, which not only affects the reaction process but also increases the cost of the catalyst.
Therefore, the above two methods are limited to a certain extent in industrial production.

Method used

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  • Method for synthesizing M acid

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Take a 10L autoclave for washing and dry it for later use. Add 5-dinitro-2,4,6-trimethylbenzenesulfonic acid (0.5mol), inorganic base anhydrous sodium carbonate (0.6mol), selenium (0.025mol), and deionized water 3L into the autoclave in turn, Introduce carbon monoxide gas to 5MPa, react at 150°C for 5 hours, stir, filter, then adjust the pH to 1 with hydrochloric acid to precipitate the product, filter with suction, and recrystallize to obtain the pure product. The highest purity of the product measured by high performance liquid chromatography is 99.9%.

Embodiment 2

[0028] Other experimental methods and conditions are with embodiment 1, only change the reaction time, record the yield of M acid as table 1:

[0029] Table 1

[0030] time (h) 2 3 4 5 6 7 Yield (%) 53.94 69.4 76.7 84.21 78.24 75.22

Embodiment 3

[0032] Other experimental method and condition are with embodiment 1, only change the kind of alkali, record the yield of M acid as table 2:

[0033] Table 2

[0034] alkali Et 3 N

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Abstract

The invention belongs to the field of chemical synthesis, and particularly relates to a method for synthesizing M acid. The method includes reacting 5-dinitro-2,4,6-trimethylbenzenesulfonic acid adopted as a raw material at a high temperature under high pressure with the presence of carbon monoxide gas by adopting water as a solvent, adopting selenium as a catalyst and adopting an alkali as a co-catalyst; performing stirring and filtration; adjusting pH with hydrochloric acid to precipitate a product; and performing suction filtration and recrystallization to obtain a target product. The moleratio of the 5-dinitro-2,4,6-trimethylbenzenesulfonic acid to the selenium is 100:2-10, the mole ratio of the 5-dinitro-2,4,6-trimethylbenzenesulfonic acid to the water is 1:111 to 1:667, and the moleratio of the 5-dinitro-2,4,6-trimethylbenzenesulfonic acid to the co-catalyst is 5:1 to 5:8. The alkali is an organic alkali or an inorganic alkali. The method adopts a high-pressure reaction in a one-pot reaction manner, and is low in equipment investment, simple and safe to operate, low in cost, capable of meeting requirements of green chemistry, economical, capable of phase transfer catalysis,and the like.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, in particular to a method for synthesizing M acid. Background technique [0002] M acid, the chemical name is 3,5-diamino-2,4,6-trimethylbenzenesulfonic acid, referred to as M acid. [0003] As an important chemical raw material, dyes play an important role in life and production, among which the dyes of bromamine blue 3R and reactive brilliant blue K-3R are in great demand at home and abroad. And M acid is exactly the important intermediate of synthesizing these two kinds of dyes, and M acid is highly selectively generated under high-pressure selenium catalysis, makes the synthesis of dye intermediate M acid more green, and more meets the needs of modern industrial production. There are two traditional reduction methods for synthesizing M acid: (1) iron powder reduction method, and (2) catalytic hydrogenation reduction method. The above two methods have their own advantages and disadvantages....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C303/22C07C309/46B01J27/057
CPCB01J27/0573C07C303/22C07C309/46
Inventor 刘晓智陈志华刘金秀
Owner LIAONING UNIVERSITY
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