Preparation process of 2-amino-4-acetyl aminoanisole

A technology of acetamidoanisole and preparation process, which is applied in the field of preparation technology of 2-amino-4-acetamidoanisole, can solve the problems of complex process, many side reactions, and high product impurity content, and achieves process safety , the effect of no three waste discharge, short process flow

Active Publication Date: 2014-01-22
SHANGHAI ZONGXING CHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] 2-Amino-4-acetylaminoanisole is used as a disperse dark blue H-GL intermediate. At present, there are not many domestic manufacturers and the output is very small. In the past, Zhejiang Huangyan United Chemical Plant and Jiaojiang Chemical No. 4 Plant had small-scale production facilities ,

Method used

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  • Preparation process of 2-amino-4-acetyl aminoanisole
  • Preparation process of 2-amino-4-acetyl aminoanisole
  • Preparation process of 2-amino-4-acetyl aminoanisole

Examples

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Example Embodiment

[0050] A preparation process of 2-amino-4-acetamido anisole,

[0051] Add accurately measured methanol, 2,4-dinitroanisole, and catalyst into the hydrogenation kettle, and perform hydrogenation reaction after low-pressure nitrogen replacement. When the system no longer absorbs hydrogen, cool, filter and recover the catalyst, and then acylate Add acetic anhydride to the kettle to carry out the acylation reaction. The temperature is controlled at 5°C. After the acylation reaction is completed, methanol is recovered through the methanol rectification tower, and the materials enter the vacuum distillation kettle to recover acetic acid. The materials in the kettle are cooled and crystallized to obtain 2-amino-4-acetamido anisole product.

[0052] The ratio of the 2,4-dinitroanisole, acetic anhydride, and catalyst is 1100:590:5. The catalyst refers to Raney nickel.

[0053] The invention can provide an output of 6000 tons / year. The project realizes a total industrial output value of 210 ...

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Abstract

The invention discloses a preparation process of 2-amino-4-acetyl aminoanisole. The preparation process comprises the following steps of (1) taking methanol as a solvent and 2,4-dimitroanisole as a raw material, introducing hydrogen to perform catalytic hydrogenation reduction reaction in the presence of a catalyst; (2) performing solid-liquid separation, and recovering the catalyst; (3) adding acetic anhydride to perform acetylation reaction; (4) recovering methanol which is recycled as a solvent for follow-up hydrogenation reduction; (5) performing reduced pressure distillation to recover acetic acid; (6) performing cooling crystallization to obtain a 2-amino-4-acetyl aminoanisole product.

Description

technical field [0001] The invention relates to the field of preparation of chemicals, in particular to a preparation process of 2-amino-4-acetamidoanisole. Background technique [0002] At present, the types of disperse dyes produced in my country are relatively complete, including high-energy type, medium-energy type, fast dyeing type, etc., with more than 150 varieties, and almost all large-tonnage varieties produced abroad are produced in my country. At present, there are 7 companies with an annual output exceeding 10,000 tons, namely, disperse dark blue H-GL, disperse blue EX-SF300%, disperse ruby ​​S-2GFL, disperse yellow brown S-2RFL, disperse red 3B / FB, disperse blue 2BLN and Disperse black EX-SF300%. Even so, many dyes are subject to the production of intermediates. For example, disperse dark blue H-GL is subject to the production of raw material 2-amino-4-acetamidoanisole, which leads to high production costs and affects the competitiveness of products in the inte...

Claims

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Application Information

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IPC IPC(8): C07C233/43C07C231/02
CPCY02P20/584
Inventor 祝梓琦
Owner SHANGHAI ZONGXING CHEM TECH CO LTD
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