A method for continuous production of 2-amino-4-acetamidoanisole
A technology for acetamidoanisole and dinitroanisole, which is applied in the field of preparation of organic compounds, can solve the problems of affecting product selectivity, excessive local proportioning, affecting product yield and the like, and achieves improved reaction safety, Accurate control of reaction temperature, reaction selectivity and high yield
Active Publication Date: 2019-04-19
HIGH & NEW TECH RES CENT OF HENAN ACAD OF SCI
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Problems solved by technology
[0009] The advantages and disadvantages of this type of method are described in detail in the patent CN105348132A, and the process of synthesizing 2-amino-4-acetamidoanisole with 2,4-dinitrochlorobenzene as raw material is optimized. This process has fewer steps , environmentally friendly, but in this batch process, due to the influence of mass transfer and heat transfer efficiency, it is easy to have local over-proportioning and local overheating problems, and it is easy to generate too many by-products if the product continues to stay in the reactor 2,4-Diacetamidoanisole affects the selectivity of the product, causing difficulty in product separation and affecting the product yield
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[0030] In order to better understand the present invention, the following examples are cited. The content described in the examples is only for illustrating the present invention, and should not and will not limit the present invention described in the claims.
[0031] Example 1-17
[0032] Combined with the accompanying drawings, a constant flow pressure pump and a nitrogen cylinder are respectively connected to a continuous flow reactor with a solid-liquid separator. First, nitrogen is introduced to replace the air in the reaction system, and then the first-stage reactor is heated to a certain level with an oil bath. Temperature, adjust the pressure of the first stage reactor to the required pressure through the back pressure valve. 2,4-Dinitroanisole and catalyst (Pd / C, 1%, particle size less than 100 microns) are added to the methanol solution, and the metering pump passes through the feed port 1, and enters the tubular continuous At the same time, hydrogen gas is introdu...
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Abstract
The invention discloses a method for continuous production of 2-amino-4-acetaminoanisole and belongs to preparation of organic compounds. According to the method, 2,4-dinitrobenzene methyl ether is used as a raw material, and the 2-amino-4-acetaminoanisole is obtained through hydrogenation reduction and selective acylation. The method adopts a continuous flow process, the phenomenon that the 2-amino-4-acetaminoanisole is in contact with air and accordingly is oxidized is avoided through strict control of raw material proportion, standing time and reaction temperature, the selective acylate 2-amino-4-acetaminoanisole is obtained at high yield, the yield is up to 99%, and the purity is up to 99.9%.
Description
technical field [0001] The invention relates to a method for preparing organic compounds, in particular to a method for continuous production of 2-amino-4-acetamidoanisole. Background technique [0002] 2‐Amino‐4‐Acetamidoanisole, commonly known as reduced substance, is an important intermediate for the preparation of Disperse Blue 79, Disperse Blue 301, and Disperse Blue 270. The traditional production process uses p-nitrochlorobenzene to produce 2-amino-4-acetamidoanisole through etherification, alkali sulfide reduction, acylation, nitration, and iron powder reduction. The chemical reaction formula is as follows: [0003] Reaction one [0004] [0005] This production process will produce a large amount of alkali sulfide reduction wastewater, iron sludge waste residue and waste acid with high concentration of organic matter. The treatment of "three wastes" is a big problem, so it has long been included in the list of backward production capacity elimination by the coun...
Claims
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IPC IPC(8): C07C231/02C07C233/43B01J19/24
CPCY02P20/584
Inventor 李中贤王俊伟刘小培殷园园董学亮余学军徐丹
Owner HIGH & NEW TECH RES CENT OF HENAN ACAD OF SCI