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Synthesis method for preparing m-aminoacetanilide hydrochloride from dinitrochlorobenzene

A technology of aminoacetanilide hydrochloride and dinitrochlorobenzene is applied in the synthesis field of dinitrochlorobenzene to prepare m-aminoacetanilide hydrochloride, and can solve problems such as low efficiency, low safety factor, and large resource consumption. , to achieve the effect of ensuring simplicity, realizing reuse, and reducing energy costs

Inactive Publication Date: 2021-09-14
徐圣杰
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this technique has successfully realized the preparation of m-phenylenediamine, yet, the reaction adopts a batch process, and the reaction time needs 4-5h, which is inefficient, and the reaction is carried out in a closed tank type, and the safety factor is low; in addition, the raw materials of the reaction It is limited to 2,4-dinitrochlorobenzene, and the refining and purification in the preparation process of 2,4-dinitrochlorobenzene still needs to consume a lot of resources

Method used

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  • Synthesis method for preparing m-aminoacetanilide hydrochloride from dinitrochlorobenzene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] The mixture of 2,4-dinitrochlorobenzene (60wt%) and 2,6-dinitrochlorobenzene (40wt%) is dissolved in methanol with a mass ratio of 1:10 to obtain the methanol of dinitrochlorobenzene solution; the methanol solution of dinitrochlorobenzene is preheated to 90 ° C, and hydrogen is continuously input into a fixed-bed microreactor for reduction hydrogenation reaction. The fixed catalyst in the reactor is platinum carbon to control the dinitrochlorobenzene The molar ratio of hydrogen is 1:8, the reaction pressure is 2.5MPa, and the reaction time is 60s; after the reaction, gas-liquid separation and recovery of hydrogen; the reduction solution is distilled under reduced pressure to recover methanol and water, and then preheated with acetic acid and hydrochloric acid to 90 ℃, then enter the reactor for acylation reaction, control the mass ratio of dinitrochlorobenzene to acetic acid and hydrochloric acid to be 1:0.5:2.5, the concentration of hydrochloric acid is 20wt%, and the r...

Embodiment 2

[0037] Dissolve 2,4-dinitrochlorobenzene in ethanol at a mass ratio of 1:5 to obtain an ethanol solution of dinitrochlorobenzene; preheat to 145°C, and continuously input hydrogen into a fixed-bed microreactor for reduction reaction. The catalyst fixed in the reactor is nickel / silicon dioxide, the molar ratio of dinitrochlorobenzene and hydrogen is controlled to be 1:10, the reaction pressure is 2MPa, and the reaction time is 80s; The solution is distilled under reduced pressure to recover ethanol and water, preheated with acetic acid and hydrochloric acid to 85°C, and then input into the reactor for acylation reaction, controlling the mass ratio of dinitrochlorobenzene to acetic acid and hydrochloric acid to be 1:0.6:2.7, The concentration was 18wt%, and the reaction time was 11 hours. After the reaction, the temperature was lowered to 15°C to precipitate solids, and the product m-aminoacetanilide hydrochloride was separated by centrifugation. The mother liquor was recovered a...

Embodiment 3

[0039]Dissolve 2,6-dinitrochlorobenzene in methanol at a mass ratio of 1:8 to obtain a methanol solution of dinitrochlorobenzene; preheat to 40°C, and continuously input hydrogen into a fixed-bed microreactor for reduction reaction. The catalyst fixed in the reactor is ruthenium carbon, the molar ratio of dinitrochlorobenzene and hydrogen is controlled to be 1:8, the reaction pressure is 4.8MPa, and the reaction time is 25s; Recover methanol and water by distillation under reduced pressure. After preheating with acetic acid and hydrochloric acid to 80°C, they are input into the reactor for acylation reaction. 22 wt%, and the reaction time is 17 hours. After the reaction, the temperature was lowered to 20°C to precipitate a solid, and the product m-aminoacetanilide hydrochloride was separated by centrifugation. The mother liquor was recovered and replaced with hydrochloric acid for the next batch of acylation reactions. The purity of the obtained m-aminoacetanilide hydrochlorid...

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Abstract

The invention discloses a synthesis method for preparing m-aminoacetanilide hydrochloride from dinitrochlorobenzene, wherein the method comprises the steps: preparing dinitrochlorobenzene and an organic solvent into a dinitrochlorobenzene solution, then feeding the dinitrochlorobenzene solution and hydrogen into a reactor for reduction reaction, and carrying out gas-liquid separation on the reacted material to recover excess hydrogen for reduction reaction; distilling the liquid material after gas-liquid separation to separate out an organic solvent and water, and then carrying out acylation reaction with acetic acid and hydrochloric acid; recovering the organic solvent separated by distillation for preparing a dinitrochlorobenzene solution; and cooling the material obtained in the acylation reaction to obtain a supersaturated solution, crystallizing to separate out aminoacetanilide hydrochloride, carrying out solid-liquid separation, recovering the mother liquor to replace part or all of hydrochloric acid, and carrying out acylation reaction with the liquid material and acetic acid. According to the method disclosed by the invention, the characteristics of seamless connection, high efficiency and coherence of upstream and downstream processes are shown from raw material acquisition and reduction to acylation reaction, the whole reaction is simple and easy to control, medium materials are recycled, and the environmental protection pressure and cost are reduced.

Description

technical field [0001] The invention relates to the technical field of fine chemicals, in particular to a synthesis method for preparing m-aminoacetanilide hydrochloride from dinitrochlorobenzene. Background technique [0002] M-Aminoacetanilide hydrochloride is a commonly used chemical raw material in the field of fine chemicals, widely used as dyes and pharmaceutical intermediates, the main purpose is to prepare reactive yellow K-RN and various disperse dyes, such as disperse violet 63:1, disperse Violet 93:1, disperse blue 183:1, etc. [0003] At present, the production process of m-aminoacetanilide hydrochloride is that m-phenylenediamine and acetic acid carry out acylation reaction in hydrochloric acid and concentrated mother liquor medium. After the reaction is completed, the material is cooled and precipitated, and the product and mother liquor are obtained through solid-liquid separation. Concentration is carried out by distillation under reduced pressure or hydroge...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/02C07C233/43C07C209/36C07C209/74C07C211/51
CPCC07C231/02C07C209/36C07C209/74C07C211/51C07C233/43
Inventor 徐圣杰殷炎
Owner 徐圣杰
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