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Method for preparing acetsalicylamide

A technology of acetylsalicylamide and salicylamide, which is applied in the field of preparation of acetylsalicylamide, can solve problems such as no research report on acetylsalicylamide, and achieve low risk and toxicity, good selectivity, and high conversion rate Effect

Inactive Publication Date: 2009-03-18
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The use of ionic liquids to catalyze the acylation of aromatic hydrocarbons has also been reported, but there is no research report on the acylation of salicylamide to prepare acetylsalicylamide

Method used

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  • Method for preparing acetsalicylamide
  • Method for preparing acetsalicylamide
  • Method for preparing acetsalicylamide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Preparation of ionic liquids

[0024] Pour triethylamine into a clean 250mL large-necked flask in a fume hood, cover with a stopper, and place the flask in an ice-water bath for cooling. Quickly add a small amount of concentrated hydrochloric acid to the flask several times, stir well to make the reaction complete and the temperature will not be too high. Due to the high toxicity of triethylamine, in order to ensure that triethylamine is fully neutralized, a slight excess of concentrated hydrochloric acid needs to be added. Stir until the solution is a single homogeneous phase and keep for 10 min. After the neutralization reaction was completed, the solution was rotated to remove most of the water under vacuum, and triethylamine hydrochloride was crystallized to obtain a white solid, which was dried at 110° C. for 24 hours for use.

[0025] Charge dry nitrogen in the anaerobic and anaerobic operation box, take the triethylamine hydrochloride prepared above in a 250mL ...

Embodiment 2

[0032] The preparation of ionic liquid is with embodiment 1.

[0033] Charge nitrogen into a 100mL dry three-neck round bottom flask, add 6ml (about 20mmol) of ionic liquid catalyst, and turn on reflux condensed water; ℃, 46℃; after the salicylamide and the ionic liquid are mixed into a uniform slurry, add 200% theoretical amount of acetyl chloride under stirring, stir well to make the mixture uniform, and start to calculate the reaction time for 2 hours. After the predetermined reaction time is reached, the heating is stopped. Quickly add 50mL of dilute hydrochloric acid (diluted 10-20 times with concentrated hydrochloric acid) to the above-mentioned three-necked round-bottomed flask to fully hydrolyze the catalyst and unreacted acetyl chloride, stir and cool to about 30°C, and precipitate solids. Transfer to a 100mL small beaker and age for 2 days. Suction filtration, washing with hydrochloric acid solution, 20 mL each time, repeated 3 times, and then washing with distille...

Embodiment 3

[0036]The preparation of ionic liquid is with embodiment 1.

[0037] In a dry 100mL three-necked round-bottomed flask, fill nitrogen, add 6ml (about 20mmol) of ionic liquid catalyst, and turn on reflux condensed water; then add 20mmol, 15mmol, and 10mmol salicylamide under stirring, and slowly heat up to 39°C; After salicylamide and ionic liquid are mixed into a uniform slurry, add 200% theoretical amount of acetyl chloride under stirring, stir well to mix evenly, and start to calculate the reaction time 1h (60min), 2h, 4h, 8h (480min) . After the predetermined reaction time is reached, the heating is stopped. Quickly add 50mL of dilute hydrochloric acid (diluted 10-20 times with concentrated hydrochloric acid) to the above-mentioned three-necked round-bottomed flask to fully hydrolyze the catalyst and unreacted acetyl chloride, stir and cool to about 30°C, and precipitate solids. Transfer to a 100mL small beaker and age for 2 days. Suction filtration, washing with hydrochl...

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Abstract

The present invention relates to a method for preparing actylamide, in particular to a novel acylation method for preparing actylamide by using triethyl ammonium-alchlor (C2H5)3NHCl-nAL3 (n is equal to 2.0 minus 2.5) ion liquid as a catalyst and a solvent to catalyze salicylamide. The method is characterized in that in the presence of nitrogen, acetyl chloride is added to undergo synthesis reaction when the temperature of the salicylamide reactant in the ion liquid rises to between 32 and 46 DEG C. The method has the advantages that the obtained actylamide is high in conversion rate, good in selectivity, and high in purity, the reaction time of the process is short, the method is economic in resources, low in risk and toxicity, low in contamination, easy to control reaction conditions, and easy and simple in the process, and the like.

Description

technical field [0001] The present invention relates to a kind of method for preparing acetylsalicylic amide, refer specifically to using triethylammonium-n aluminum trichloride (C 2 h 5 ) 3 NHCl-nAlCl 3 (n=2.0-2.5) as a catalyst, and catalyzes a new method for preparing acetylsalicylicamide by acylation of salicylamide. Background technique [0002] 5-acetylsalicylamide (5-acetylsalicylamide, abbreviated as: 5-ASA, molecular formula C 9 h 9 NO 3 ) is white or beige powder, odorless, tasteless, non-toxic, insoluble in water. 5-Acetylsalicylamide is an important pharmaceutical intermediate, which is used to synthesize the cardiovascular drug Raberol, and can also be further synthesized to 5-bromoacetylsalicylamide, which is used to synthesize and treat allergic and morbid diseases such as asthma , Allergic rhinitis, tuberculosis membrane, urticaria, eczema, high blood pressure and other drugs. [0003] The traditional synthesis process of 5-acetylsalicylamide is to us...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C235/60C07C231/14
CPCY02P20/54
Inventor 殷恒波陈维广祝久庚王仲文姜廷顺
Owner JIANGSU UNIV
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