A method for preparing 2-(4-carbamoylmethyl-phenyl)-acetamide by amidation of diacetophenone

A technology of carbamoylmethyl and diacetyl benzamide, which is applied to the preparation of carboxylic acid amide, chemical instruments and methods, and the preparation of organic compounds, etc., can solve the problems of diethylbenzene overcapacity and overcapacity, and reduce the Product separation difficulty and energy consumption, short reaction time, high conversion effect

Active Publication Date: 2020-11-10
SINOPEC YANGZI PETROCHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Sinopec Yangzi Petrochemical successfully developed the process of producing high-purity p-diethylbenzene by adsorption method, but there is a problem of overcapacity in high-purity p-diethylbenzene. This invention uses para-diacetophenone, an oxidation product of p-diethylbenzene, as raw material , can solve the problem of excess production capacity of p-diethylbenzene, but there is no report on the process of preparing 2-(4-carbamoylmethyl-phenyl)-acetamide by amidation of p-diacetophenone as a raw material, so the development of p-diacetyl The synthesis process of 2-(4-carbamoylmethyl-phenyl)-acetamide by direct amidation of benzene has far-reaching significance

Method used

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add the p-diacetophenone of 1mmol in the autoclave, aminating agent is ammoniacal liquor, vulcanizing agent is sulfur, solvent is ethanol, the mol ratio of aminating agent and p-diacetophenone is 10, the ratio of vulcanizing agent and p-diacetophenone The molar ratio is 10, and the mass ratio of solvent to p-diacetophenone is 20. When the reaction temperature is 160° C., the reaction pressure is 1.6 MPa, and the reaction time is 4 hours, the conversion rate of p-diacetophenone is 84.46%. 2-(4- The yield of carbamoylmethyl-phenyl)-acetamide was 59.12%.

Embodiment 2

[0027] Add 1 mmol of p-diacetophenone in the autoclave, the aminating agent is ammonium bicarbonate, the vulcanizing agent is ammonium sulfide, the solvent is ethanol, the molar ratio of aminating agent to p-diacetophenone is 10, the vulcanizing agent and p-diacetophenone The molar ratio of acetophenone is 16, and the mass ratio of solvent to p-diacetophenone is 60. When the reaction temperature is 160° C., the reaction pressure is 1.0 MPa, and the reaction time is 3 hours, the conversion rate of p-diacetophenone is ~100.00%. 2 The yield of -(4-carbamoylmethyl-phenyl)-acetamide was 71.63%.

Embodiment 3

[0029] Add 1 mmol of p-diacetophenone in the autoclave, the aminating agent is urea, the vulcanizing agent is sodium sulfide, the solvent is DMF, the molar ratio of aminating agent to p-diacetophenone is 12, the vulcanizing agent and p-diacetophenone The mol ratio is 16, and the mass ratio of solvent and p-diacetophenone is 60, and when reaction temperature 140 ℃, reaction pressure 1.0MPa, reaction time 4h, record p-diacetophenone transformation efficiency 90.65%, 2-(4 -Carbamoylmethyl-phenyl)-acetamide yield 61.39%.

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Abstract

The present invention relates to a method for preparing p-benzene diacetamide through amidation of p-diacetylbenzene. According to the present invention, p-diacetylbenzene is used as a raw material, an aminating agent, a vulcanizing agent and a solvent are added, and a reaction is performed at a reaction temperature of 80-180 DEG C under a reaction pressure of 0.5-2.0 MPa to obtain the product p-benzene diacetamide; and the method has advantages of simple operation, high p-diacetylbenzene conversion rate, high p-benzene diacetamide yield, non-toxic raw material, high reaction safety, high economic benefit, broad industrial application prospect and the like, and can avoid the use of nitrile substances.

Description

technical field [0001] The invention relates to a method for preparing 2-(4-carbamoylmethyl-phenyl)-acetamide through amidation of diacetophenone, belonging to the technical field of fine chemicals. Background technique [0002] 2-(4-carbamoylmethyl-phenyl)-acetamide (p-benzonediacetamide, CAS No: 30038-76-7) is an important organic intermediate, mainly used in medicine and other fields. At present, the main synthesis method of 2-(4-carbamoylmethyl-phenyl)-acetamide is concentrated acid hydrolysis and alkali washing process of nitriles. Nitriles are usually obtained by reacting benzyl chloride and sodium cyanide in aqueous dimethylamine solution. Nitriles were stirred and dissolved in concentrated hydrochloric acid or concentrated sulfuric acid, and reacted at 50°C for 0.5h. After cooling, filtering and washing with ice water, the crude product was obtained. The crude product was washed with sodium carbonate solution, then with ice water, and dried to obtain a relatively ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C231/10C07C233/11
CPCC07C231/10C07C233/11
Inventor 仲文徐向荣许如霞任红锋王海燕刘石伟崔群高嵩
Owner SINOPEC YANGZI PETROCHEM
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