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Synthetic method of m-amino acetanilide

A technology for the synthesis of aminoacetanilide and its synthesis method, which is applied in the field of synthesis of m-aminoacetanilide, can solve the problems of long cycle, high energy consumption, and cumbersome steps, and achieve the effects of short production cycle, low energy consumption, and simple process

Inactive Publication Date: 2008-12-24
浙江龙盛染料化工有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The concentrated hydrochloric acid in the above method is volatile, and in the synthesis process, the mother liquor needs to be used in the next batch after vacuum distillation and other links, which has problems such as cumbersome steps, not easy to operate, high energy consumption, and long cycle.

Method used

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  • Synthetic method of m-amino acetanilide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Get m-acetamidoaniline mother liquor 660g, wherein contain: hydrochloric acid 33g, acetic acid 59.4g, m-acetamidoaniline 30g, m-phenylenediamine 50g, m-diacetamidoaniline 60g, pass into HCl gas 30g by differential method at normal temperature, Add 88g of m-phenylenediamine and 56g of glacial acetic acid (percentage), heat up to 96-104°C and react for 20h, cool down to below 35°C and filter, drain the obtained filter cake, add 20g of water to wash, and obtain a purity of 99 % m-acetamido aniline, washing liquid and mother liquor mix about 680g, as the mother liquor of applying mechanically next time.

Embodiment 2

[0024] Take 660g of mother liquor, which contains: 59.4g of hydrochloric acid, 105g of acetic acid, 44g of m-phenylenediamine, 80g of m-phenylenediamine, 25g of HCl gas by differential method at normal temperature, and add m-phenylenediline 88 g of amine and 56 g of glacial acetic acid (100 percent), heated up to 96-104 ° C for 20 hours, cooled to below 35 ° C and filtered, after the obtained filter cake was drained, 30 g of water was added to wash, and the purity of 99% m-acetyl Aminoaniline, lotion and mother liquor mix about 690g, as the mother liquor of applying mechanically next time.

Embodiment 3

[0026] Get the lotion that obtains of embodiment 2 and mother liquor 690g, wherein contain: hydrochloric acid 45.4g, acetic acid 75g, m-acetamidoaniline 40g, m-phenylenediamine 60g, m-diacetamidoaniline 70g, pass through differential method at normal temperature Add 28g of HCl gas, add 88g of m-phenylenediamine and 28g of acetic anhydride (100%), heat up to 110-118°C and react for 18h, cool down to below 35°C and filter, drain the obtained filter cake, add 25g of water to wash , to obtain a purity of 99% m-acetaminoaniline, washing liquid and mother liquor mixed about 690g, as the next time the mother liquor.

[0027] Analysis shows that adopting the process of the invention can not only simplify operation and save energy, but also has no slight influence on the purity of the product.

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Abstract

The invention provides a method for synthesizing m-Aminoacetanilide. Compared with the prior method for synthesizing m-Aminoacetanilide, the method is characterized in that chlorine hydride gas replaces hydrochloric acid with a content of 31 percent, the step of concentrating a mother liquid in the subsequent steps is avoided, a large number of production resources and the cost are saved, the final reaction liquid is pumped and filtered to remove the product, the filter liquor can be reused for the next reaction immediately, and the step of concentrating the mother liquid is not needed; and the process is simple, the production cycle is short and the energy consumption is low.

Description

(1) Technical field [0001] The invention relates to a synthesis method of m-aminoacetanilide. (2) Background technology [0002] M-Aminoacetanilide is a widely used chemical raw material. It is widely used as an intermediate of fast dyes and medicines, and is mainly used to prepare reactive yellow K-RN and disperse dyes. It is in great demand. [0003] In the synthesis process of m-aminoacetanilide, the general production process uses acetic acid (or acetic anhydride), hydrochloric acid (31% content), m-phenylenediamine, and the mother liquor of the last cycle after concentration, heated to 90°C After the reaction, the material is cooled to about 20°C through the condensing medium, and the product is obtained by suction filtration. The mother liquor obtained after separation is collected, and the mother liquor water is concentrated by vacuum distillation, and the water in the mother liquor is removed. (During the vacuum distillation process, since acetic acid and water form...

Claims

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Application Information

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IPC IPC(8): C07C233/07C07C231/02
Inventor 欧其高怀庆倪嵩涛姜兴中
Owner 浙江龙盛染料化工有限公司
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