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Microwave synthesis method of 3-[N-(4-nitrophenyl)-amido] propionic acid

A technology for nitrophenyl and microwave synthesis, which is applied in the preparation of carboxylic acid amides, chemical instruments and methods, and the preparation of organic compounds, to achieve the effects of simplifying the reaction process, increasing yield, and saving resources

Inactive Publication Date: 2012-12-26
HENAN AGRICULTURAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But utilize the method of microwave synthesis 3-[N-(4-nitrophenyl-amido] propionic acid, also do not see report both at home and abroad

Method used

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  • Microwave synthesis method of 3-[N-(4-nitrophenyl)-amido] propionic acid
  • Microwave synthesis method of 3-[N-(4-nitrophenyl)-amido] propionic acid
  • Microwave synthesis method of 3-[N-(4-nitrophenyl)-amido] propionic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Weigh 1.38g of p-nitroaniline and 0.98g of succinic anhydride, mix and grind them evenly into powder, add dropwise 0.5mL of glacial acetic acid, mix quickly, microwave 1000W for 20s~5min, cool naturally, add 4mL of tap water to wash repeatedly, and filter with suction , and the filtrate was dried naturally to obtain the target product 3-[N-(4-nitrophenyl)-amido]propionic acid, melting point: 192-194° C., yield 91.42%. The synthetic route is as follows.

[0020]

[0021] 3-[N-(4-nitrophenyl)-amido]propionic acid synthesis route

example 2

[0023] Weigh 1.38g of p-nitroaniline and 0.10g of succinic anhydride and dissolve them in 0.2mL of acetic acid, mix quickly, irradiate with 800W microwave for 3-5min, cool naturally, after 30min, add 4mL of tap water to wash repeatedly, suction filter, suction filter The product was dried naturally to obtain the target product 3-[N-(4-nitrophenyl)-amido]propionic acid with a yield of 92.3%.

example 3

[0025] Weigh 13.8g of p-nitroaniline and 10g of succinic anhydride, mix and grind them evenly into powder, place them in a microwave reactor for 10 minutes of continuous radiation at 500W, add 4 mL of glacial acetic acid dropwise, mix quickly, microwave 500W for 10 seconds to 5 minutes, and cool naturally , adding 10 mL of tap water for repeated washing, suction filtration, and natural drying of the filtrate to obtain the target product 3-[N-(4-nitrophenyl)-amido]propionic acid with a yield of 90.62%.

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Abstract

The invention discloses a microwave synthesis method of 3-[N-(4-nitrophenyl)-amido] propionic acid, which is synthesized in the following steps that: microwave synthesis is carried out to nitroaniline and succinic anhydride in a microwave reactor with the microwave frequency of 500 to 1000w, the internal pressure of a microwave oven of 0.1 to 0.4MPa and the microwave irradiation time of 10s to 20min when the organic solvent serves as a reaction medium, to prepare 3-[N-(4-nitrophenyl)-amido] propionic acid solution; and the solution is purified and naturally dried to prepare the 3-[N-(4-nitrophenyl)-amido] propionic acid. By adopting the technical scheme, the invention has the advantages that the microwave synthesis method of 3-[N-(4-nitrophenyl)-amido] propionic acid does not need a large amount of solution and does not need to add any catalyst during the reaction, has relatively simple purification process because the amount of solution is little and no catalyst exists, greatly improves the yield, greatly simplifies the reaction process, and is a high-efficiency, time and resource saving synthesis method.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, in particular to a method for synthesizing 3-[N-(4-nitrophenyl)-amido]propionic acid. Background technique [0002] 3-[N-(4-nitrophenyl)-amido]propionic acid is an important intermediate in organic synthesis. It can not only be linked to protein carriers as a complete antigen for the preparation of antibodies against it, but also its metal tin-derived The substance has biological activity such as inhibiting bacillus and fungi. Ross.Biere of the United States Department of Agriculture reported the synthesis of 3-[N-(4-nitrophenyl)-amido]propionic acid in 2001 by dissolving p-nitroaniline and succinic anhydride in ethyl acetate Add lutidine to the ester as a catalyst, stir and react at 70°C for 19 hours, pour off the solvent after the reaction, and purify the crude product by thin-layer chromatography, and then by high-performance liquid chromatography, with a yield of 59%. This method ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C233/15C07C231/02
Inventor 宁长申杨国玉陈龙飞菅复春张龙现乔亚辉齐萌
Owner HENAN AGRICULTURAL UNIVERSITY