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A kind of synthetic method of m-aminoacetanilide hydrochloride

A technology of aminoacetanilide hydrochloride and synthesis method, which is applied in the field of synthesis of m-aminoacetanilide hydrochloride, can solve the problems of high energy consumption, long reaction cycle, high reaction temperature, etc., and achieve high yield and product yield High, easy-to-operate effect

Active Publication Date: 2020-08-28
YANTAI ANOKY FINE CHEM CO LTD +4
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by this invention is to provide a kind of synthetic method of m-aminoacetanilide hydrochloride in order to overcome the problems of high reaction temperature, long reaction cycle and high energy consumption in the prior art. The method adopts acetic anhydride as The reaction reagents react at low temperature, and crystals are precipitated while reacting, which reduces the crystallization cooling process, greatly reduces the energy consumption of the whole process, and the mother liquor can be directly applied to the next batch without distillation and concentration process, and the steps are simplified

Method used

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  • A kind of synthetic method of m-aminoacetanilide hydrochloride
  • A kind of synthetic method of m-aminoacetanilide hydrochloride

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Stir and add 150g of 50% acetic acid into a 500ml four-necked bottle, stir and add 54.0g of m-phenylenediamine, and add 59.88g of hydrochloric acid (32%) dropwise at 15-25°C for 30 minutes, stir until the material dissolves, and then cool down in an ice bath to 0-25°C. 5°C. Add 53.6g of acetic anhydride at 0~5°C over 4~5h. After the addition, the reaction was continued at this temperature for 1 hour, and sampling was carried out. The raw materials were 0.71%, m-aminoacetanilide hydrochloride 90.2%, m-diacetanilide hydrochloride 8.04%, filtered to obtain m-aminoacetanilide hydrochloride wet cake 96.3g , purity 98.91%, amino value 84.57%, yield 88.21%, mother liquor 205.3g (raw material 14.23%, m-aminoacetanilide hydrochloride 35.76%, m-diacetanilide 47.5%) is used in the next batch.

Embodiment 2

[0027] Add 150 g of the mother liquor in Example 1 into the flask, add 59.88 g of hydrochloric acid (32%), stir and heat up to 80° C. Insulate at 80-90°C for 1h. Cool down to 60°C, take samples to detect the content of hydrochloric acid and acetic acid, the content of hydrochloric acid is 10.4%, and the content of acetic acid is 40.1%. Add 54g of m-phenylenediamine, stir to dissolve, and lower the temperature to 0-5°C at the same time. Add 58.3g of acetic anhydride dropwise over 4 to 5 hours, and keep warm at 0 to 5°C for 1 hour after the addition, and detect that the raw material is 0.32%, m-aminoacetanilide hydrochloride is 91.61%, and m-diacetanilide is 7.84%. After the end point, filter to obtain m-aminoacetanilide hydrochloride wet cake 107.5g, purity 99.0%, amino value 84.25%, yield 98.10%, mother liquor 190.2g (raw material 15.65%, m-aminoacetanilide hydrochloride 37.16%, Between diacetamidoaniline 46.22%) cover for next batch.

Embodiment 3

[0029] Add 150 g of the mother liquor in Example 2 into the flask, add 59.88 g of hydrochloric acid (32%), stir and heat up to 80° C. Insulate at 80-90°C for 1h. Cool down to 60°C, take samples to detect the content of hydrochloric acid and acetic acid, the content of hydrochloric acid is 10.7%, and the content of acetic acid is 39.5%. Add 54g of m-phenylenediamine, stir to dissolve, and lower the temperature to 0-5°C at the same time. Add 58.3g of acetic anhydride dropwise over 4 to 5 hours, and keep warm at 0 to 5°C for 1 hour after the addition, and detect that the raw material is 0.51%, m-aminoacetanilide hydrochloride is 90.47%, and m-diacetanilide is 8.52%. After the end point, filter to obtain 107.7g of m-aminoacetanilide hydrochloride wet cake, with a purity of 98.93%, an amino value of 84.42%, and a yield of 98.48%. The mother liquor 187.1g is used in the next batch.

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Abstract

The invention discloses a method for synthesizing 3'-aminoacetanilide hydrochloride. The method comprises the following steps: dropwise adding acetic anhydride into a mixed solution of m-phenylenediamine and hydrochloric acid in an acetic acid aqueous solution at 0-5 DEG C, and keeping the temperature to perform a reaction as shown in the specification. According to the synthesizing method, aceticanhydride is adopted as a reacting reagent to react at a low temperature, crystal is separated during the reaction, so that the process of crystallizing and cooling is reduced, energy consumption inthe whole process can be greatly reduced, and the stock solution can be directly used in next batch without a distilling or concentrating process, so that the steps can be simplified.

Description

technical field [0001] The invention relates to a synthesis method of m-aminoacetanilide hydrochloride. Background technique [0002] M-aminoacetanilide hydrochloride is a very important intermediate of disperse dye coupling components, which can be used to prepare disperse dyes such as 93# purple coupling components. When using m-aminoacetanilide hydrochloride, use 30% liquid caustic soda can neutralize hydrochloride. [0003] The synthesis of m-aminoacetanilide hydrochloride, the existing process is to use acetic acid to react at 90 ~ 110 ° C, the reaction temperature is high, the energy consumption is large, after the reaction, it needs a long cooling crystallization process, and the obtained mother liquor needs to be extracted by vacuum distillation Concentrated and applied to the next batch, the steps are cumbersome and the energy consumption is high. Contents of the invention [0004] The technical problem to be solved by this invention is to provide a kind of synt...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C231/02C07C233/43
Inventor 曲美君刘云龙刘祥庆王乐明
Owner YANTAI ANOKY FINE CHEM CO LTD