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Production process of 2-amino-4-acetamidophenyl ether

A technology of acetamidophenyl ether and acetamidoanisole, which is applied in the field of fine chemical raw material preparation, can solve the problems of large amount of solid waste and liquid waste, long reaction cycle, large material consumption, etc., and achieves the convenience of automatic control, Good yield and reduced consumption

Pending Publication Date: 2020-06-12
中卫市鑫三元化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0022] In summary, there is a long reaction cycle in the existing production technology of 2-amino-4-acetylaminophenyl ether, wherein the consumption of materials is relatively large, and the p-nitroanisole and sodium p-nitrophenolate of the reaction product The amount of the mixture is large, and a large amount of waste water is generated when the two are separated. The treatment cost of this waste water is high, and the amount of solid waste and liquid waste is large.

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  • Production process of 2-amino-4-acetamidophenyl ether
  • Production process of 2-amino-4-acetamidophenyl ether

Examples

Experimental program
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Effect test

Embodiment 2

[0042] At room temperature, add 2,500 grams of N,N-dimethylformamide described above into a closed acylation tank with cooling, stirring, and then add 500 grams of 2,4-diaminoanisole to dissolve it , Stir for 10-15 minutes, after the dissolution is complete, start to seal and fill with nitrogen, replace the air under a slight positive pressure, and start to cool down. When the material in the reactor drops to -10~-5°C, start adding acetic anhydride, and it is expected to add 350 grams of acetic anhydride within 2 hours. After the addition of acetic anhydride, stir for 15 minutes, start to slowly raise the temperature to 30°C, turn on the vacuum pump to extract the acetic acid produced by the reaction under negative pressure, and then raise the temperature to 70°C to extract the added solvent to obtain the product. Analysis by liquid phase (HPLC) chromatography: 2-amino-4-acetamidoanisole 95.1%; 2,4-diaminoanisole 2.3%; 2,4-diacetamidoanisole 1.9%; others 0.7%.

Embodiment 3

[0044] At room temperature, add 50 kg of N,N-dimethylformamide mentioned above into a closed acylation tank with cooling, stirring, and then add 300 kg of 2,4-diaminoanisole to dissolve it , Stir for 10-15 minutes, after the dissolution is complete, start to seal and fill with nitrogen, replace the air under a slight positive pressure, and start to cool down. When the material in the reactor drops to -10~-5°C, start adding acetic anhydride, and it is expected to add 36.9 kg of acetic anhydride within 2 hours. After the addition of acetic anhydride, stir for 15 minutes, start to slowly raise the temperature to 30°C, turn on the vacuum pump to extract the acetic acid produced by the reaction under negative pressure, and then raise the temperature to 70°C to extract the added solvent to obtain the product. Analysis by liquid phase (HPLC) chromatography: 2-amino-4-acetamidoanisole 95.6%; 2,4-diaminoanisole 1.9%; 2,4-diacetamidoanisole 1.8%; others 0.7%.

[0045] The production t...

Embodiment 1

[0047] At room temperature, add 200 grams of the aforementioned N,N-dimethylacetamide into a closed acylation tank with cooling, stirring, and then add 50 grams of 2,4-diaminophenetole to dissolve it. Stir for 10 to 15 minutes, after the dissolution is complete, start to seal and fill with nitrogen, replace the air under a slight positive pressure, and start to cool down. When the material in the reactor drops to -10~-5°C, start adding acetic anhydride, and it is expected to add 36.9 grams of acetic anhydride within 2 hours. After the addition of acetic anhydride, stir for 15 minutes, start to slowly raise the temperature to 30°C, turn on the vacuum pump to extract the acetic acid produced by the reaction under negative pressure, and then raise the temperature to 70°C to extract the added solvent to obtain the product. Analysis by liquid phase (HPLC) chromatography: 2-amino-4-acetamidoanisole 95.1%; 2,4-diaminophenetole 1.8%; 2,4-diacetamidophenetole 1.9%; others 1.2% .

[0...

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Abstract

The invention belongs to the technical field of fine chemical raw material preparation, and particularly relates to a production process of 2-amino-4-acetamidophenyl ether. The method comprises the following specific production steps: weighing a solvent, adding the solvent into an acylation kettle which has cooling, stirring and sealing functions, weighing 2,4-diaminophenyl ether again, adding the2,4-diaminophenyl ether into the acylation kettle, stirring the mixture for 10-15 minutes for dissolution in the solvent; closing a feed port and a discharge port of the acylation kettle, introducingnitrogen into the acylation kettle in a closed environment, replacing air, reducing the temperature of the acylation kettle to -10 to -5 DEG C, starting to add acetic anhydride, adding 74-36.9 kg ofacetic anhydride within 1-3 hours, stirring for 10-20 minutes, and slowly heating to 25-35 DEG C; opening a vacuum pump, pumping out acetic acid generated by the reaction under negative pressure, raising the temperature of the acylation kettle to 60-80 DEG C, and pumping out the added solvent to obtain the product. The production process is safe and reliable, no side reaction condition is formed,and the purity of the obtained product is high.

Description

Technical field: [0001] The invention belongs to the technical field of preparation of fine chemical raw materials, and in particular relates to a production process of 2-amino-4-acetylaminophenyl ether. Background technique: [0002] At present, there are two production methods of 2-amino-4-acetylaminophenyl ether in China: [0003] The first is the pressure etherification method: first add molten p-nitrochlorobenzene and methanol to the reactor, heat it to 70°C under stirring, and slowly add methanol solution of sodium hydroxide with an excess concentration of 13.5% within 10 hours . Feed under reflux for 1-4h, the temperature is controlled at about 70°C; 5-8h is a pressurized reaction; the temperature is raised by 5°C per hour, the temperature rises to 92.5°C within 9h, and rises to 95°C within 10h, and the feed is completed. Stir at this temperature for 2 hours, and the sample analysis freezing point ≥ 49 ° C is qualified; then the whole methanol is removed, washed wit...

Claims

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Application Information

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IPC IPC(8): C07C231/02C07C233/43
CPCC07C231/02C07C233/43
Inventor 司马天龙周羿赵峻
Owner 中卫市鑫三元化工有限公司