Method for preparing 2-amino-4-acetaminoanisole

A technology of acetamidoanisole and amino group, applied in the chemical industry, can solve problems such as high risk factor, potential safety hazard, increase product cost, etc., and achieve the effect of simple process

Active Publication Date: 2016-12-21
ZHEJIANG RUNTU INST
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The current hydrogenation reduction preparation method of 2-amino-4-acetamidoanisole is the catalytic hydrogenation method of conventional organic solvents such as methanol. Since organic solvents such as methanol are flammable and explosive, it is dangerous under the condition of high reaction pressure. The coefficient is high, and there are great hidden dangers in terms of safety; and it is necessary to add a step of methanol recovery process, which requires huge energy consumption, and the distilled waste water also needs further treatment, which increases the cost of the product

Method used

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  • Method for preparing 2-amino-4-acetaminoanisole

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Embodiment 1

[0033] A method for preparing 2-amino-4-acetamidoanisole by hydrogenation reduction of 2-nitro-4-acetamidoanisole in water phase, in a closed reaction kettle, adding 2-nitro-4-acetamido Anisole 50g, water 500mL, Raney nickel 5g, stir and add acid-binding agent liquid caustic soda (3%) to adjust the pH value to 7.5, heat up to 95 ° C, when the system pressure drops to 2.0MPa, open the hydrogen valve, keep The hydrogen pressure is 3.0MPa. After reacting for 3-4 hours under this pressure and temperature condition, close the hydrogen valve and observe the pressure change in the kettle. If the pressure drops, continue to feed hydrogen until there is no pressure change. After the reaction, stop heating, filter while it is hot, separate and recover the catalyst, filter the filtrate to obtain 2-amino-4-acetamidoanisole after cooling and precipitation, and obtain 41.7g light brown granular product, 2-amino-4-acetamidobenzene The purity of methyl ether is 99.38%, the content is 96.67%, ...

Embodiment 2

[0035] A method for preparing 2-amino-4-acetamidoanisole by hydrogenation reduction of 2-nitro-4-acetamidoanisole in water phase, in a closed reaction kettle, adding 2-nitro-4-acetamido Anisole 50g, water 600mL, Raney nickel 5g, stir and add acid-binding agent liquid caustic soda (3%) to adjust the pH value to 7.5, heat up to 95 ° C, when the system pressure drops to 2.0MPa, open the hydrogen valve, keep The hydrogen pressure is 3.0MPa. After reacting for 3-4 hours under this pressure and temperature condition, close the hydrogen valve and observe the pressure change in the kettle. If the pressure drops, continue to feed hydrogen until there is no pressure change. After the reaction, stop heating, filter while it is hot, separate and recover the catalyst, filter the filtrate to obtain 2-amino-4-acetamidoanisole after cooling and precipitation, and obtain 41.3g of light brown granular product, 2-amino-4-acetamidobenzene The purity of methyl ether is 99.24%, the content is 96.73...

Embodiment 3

[0037] A method for preparing 2-amino-4-acetamidoanisole by hydrogenation reduction of 2-nitro-4-acetamidoanisole in water phase, in a closed reaction kettle, adding 2-nitro-4-acetamido Anisole 50g, water 500mL, Raney nickel 5g, stir and add acid-binding agent soda ash to adjust the pH value to 7.5, heat up to 95°C, when the system pressure drops to 2.0MPa, open the hydrogen valve to keep the hydrogen pressure at 3.0MPa After reacting for 3-4 hours under this pressure and temperature condition, close the hydrogen valve and observe the pressure change in the kettle. If the pressure drops, continue to feed hydrogen until there is no pressure change. After the reaction, stop heating, filter while it is hot, separate and recover the catalyst, filter the filtrate to obtain 2-amino-4-acetamidoanisole after cooling and precipitation, and obtain 41.7g light brown granular product, 2-amino-4-acetamidobenzene The purity of methyl ether is 99.28%, the content is 96.71%, and the product y...

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Abstract

The invention relates to a method for preparing 2-amino-4-acetaminoanisole, and the method belongs to the technical field of hydrogenation reduction reaction of 2-nitro-4-acetaminoanisole. In a reaction system with water as a solvent, under a condition of the presence of an acid binding agent and a catalyst, 2-nitro-4-acetaminoanisole is subjected to catalytic hydrogenation reduction into 2-amino-4-acetaminoanisole, solid-liquid separation is performed to recycle a catalyst, and cooling crystallization is performed to obtain 2-amino-4-acetaminoanisole; compared with a conventional method with an organic solvent as a reaction solvent, the production method is more environmentally friendly and lower in cost under conditions of maintaining the yield and the product purity.

Description

technical field [0001] The invention relates to a preparation method of 2-amino-4-acetylaminoanisole, which belongs to the field of chemical industry. Background technique [0002] 2-Amino-4-acetamidoanisole [0003] (CAS: 6375-47-9, 2-Amino-4-acetaminoanisole, molecular weight: 180.2) [0004] The structural formula is as follows: [0005] [0006] 2-Amino-4-acetamidoanisole is an important intermediate in the production of dyes and medicines. It is mainly used as an intermediate of disperse dyes, and it is also used in the synthesis of acid dyes, reactive dyes and pigments, and occupies an important position in the industry. Mainly used for Disperse Blue 79 # 、291 # And so on, has a larger market at home and abroad. [0007] The current hydrogenation reduction preparation method of 2-amino-4-acetamidoanisole is the catalytic hydrogenation method of conventional organic solvents such as methanol. Since organic solvents such as methanol are flammable and explosive, i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/12C07C233/43
CPCC07C231/12C07C233/43Y02P20/584
Inventor 赵国生龚斌彬阮光栋任闻飞邬伟国
Owner ZHEJIANG RUNTU INST
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