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Preparation method for gold nanometer catalyst, and obtained catalyst product and application thereof

A gold nano-catalyst technology, applied in the field of chemical catalytic synthesis, can solve the problems of unavailable quinazolines, explosives, and limited product 2-arylquinazolines, and achieve a wide range of substrates without reducing the yield Effect

Active Publication Date: 2016-02-17
UNIV OF SCI & TECH OF CHINA
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

However, unfortunately, the traditional method is to form quinoline compounds in one step by oxidative condensation of o-aminoacetophenone and benzylamine in the presence of strong oxidizing agents (Chem. Commun., 2010, 46, 5244-5246; Chem. Commun., 2011, 47, 7818–7820; Angew. Chem. Int. Ed. 2012, 51, 8077–8081)
These methods all use some excessive oxidizing agents, such as tert-butyl hydroperoxide, which are prone to explosion and bring some unsafe factors in the actual production process.
At the same time, the biggest problem is that the products prepared by these methods are often limited to 2-aryl quinazolines, and the quinazolines substituted by the 2-position are not available.
Therefore, the prospect of its application is greatly affected

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  • Preparation method for gold nanometer catalyst, and obtained catalyst product and application thereof
  • Preparation method for gold nanometer catalyst, and obtained catalyst product and application thereof
  • Preparation method for gold nanometer catalyst, and obtained catalyst product and application thereof

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[0051] More specifically, in one aspect, the invention discloses a method for preparing a gold nanocatalyst, comprising the following steps:

[0052] a) dispersing the gold source compound and the nano-template agent in a solvent;

[0053] b) adding a base to the mixture obtained in step a) to adjust its pH to 6.5-11, and then reacting at a temperature of 70-100°C for 2-5h;

[0054] c) filtering the reaction mixture obtained in step b), and vacuum-drying the filter cake at 60-100°C;

[0055] d) calcining the dried product obtained in step c) at a temperature of 250-400° C. for 1-4 hours, thereby obtaining the gold nano-catalyst.

[0056] The preferred gold source compound in the present invention is potassium chloroaurate, sodium chloroaurate, gold chloride or potassium dicyanoalloyate. Preferred nano templates are titanium dioxide, zinc oxide, activated carbon, zirconium dioxide or polyvinylpyrrolidone. Since different nano-template agents have different effects on gold na...

Embodiment 1

[0073] In a clean 50 ml round bottom flask, 1 g of zinc oxide was dispersed in 20 ml of deionized water, then 8 mg of chloroauric acid tetrahydrate was added, and then sodium carbonate was slowly added to adjust the pH of the system to about 7.0. Afterwards, a condensing reflux tube was installed and the temperature was raised to 100°C for 4 hours of reaction. After cooling to room temperature, the reaction mixture was filtered through a filter, and the obtained filter cake was washed with water, and the filter cake was dispersed in water by ultrasonic and detected by adding silver nitrate until there was no chloride ion. Next, the filter cake was vacuum dried at 90°C for 4 hours, followed by calcination in a muffle furnace at 400°C for 3 hours. The gold nanocatalyst supported by zinc oxide can be obtained, and the weight is about 810 mg. Through transmission electron microscopy and inductively coupled plasma analysis, the size of the gold catalyst is about 10nm, and the load...

Embodiment 2

[0075] In a clean 50 ml round bottom flask, 1 g of zirconium dioxide was dispersed in 20 ml of deionized water, then 8 mg of chloroauric acid tetrahydrate was added, and then sodium carbonate was slowly added to adjust the pH of the system to about 7.0. Afterwards, a condensing reflux tube was installed and the temperature was raised to 100°C for 4 hours of reaction. After cooling to room temperature, the reaction mixture was filtered through a filter, and the obtained filter cake was washed with water, and the filter cake was dispersed in water by ultrasonic and detected by adding silver nitrate until there was no chloride ion. Next, the filter cake was vacuum dried at 90°C for 4 hours, followed by calcination in a muffle furnace at 400°C for 3 hours. The gold nanocatalyst supported by zirconia can be obtained, and the weight is about 780 mg. Through transmission electron microscopy and inductively coupled plasma analysis, the size of the gold catalyst is about 6nm, and the ...

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Abstract

The invention relates to a preparation method for a gold nanometer catalyst. The preparation method comprises the following steps: dispersing a gold-source compound and a nanometer template in a solvent; adding alkali into a reaction product obtained in the previous step to adjust the pH value of the reaction product and carrying out heating so as to allow the reaction product to react with the alkali; and subjecting a product obtained in the previous step to filtering and subjecting the obtained filter cake to vacuum drying and then to calcining so as to obtain the gold nanometer catalyst. The invention also relates to a synthetic method for a quinazoline compound. The quinazoline compound is prepared by subjecting a hydrogen acceptor, a hydrogen donor, a nitrogen source and the gold nanometer catalyst to a reaction in an inert atmosphere, e.g., a nitrogen atmosphere. The gold nanometer catalyst provided by the invention has high efficiency, is repeatedly usable and can be used for catalytic preparation of the quinazoline compound.

Description

technical field [0001] The invention belongs to the field of chemical catalytic synthesis. Specifically, the present invention relates to the preparation of a metal nanoparticle and its application in the synthesis of quinazoline compounds. Background technique [0002] Quinazoline compounds exist in a large number in nature, including biomacromolecules, drug molecules and natural products, and it is the most important type of organic compounds. Quinazoline compounds have a wide range of uses, and can be used as intermediates for pesticides, spices, and medicines, and monomers for synthesizing biologically active molecules such as proteins and functional materials. [0003] Due to the importance of quinazoline compounds, they are widely concerned by the chemical, biological and medical circles. However, unfortunately, the traditional method is to form quinoline compounds in one step by oxidative condensation of o-aminoacetophenone and benzylamine in the presence of strong ...

Claims

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Application Information

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IPC IPC(8): B01J23/66B01J23/52B01J31/06C07D239/74
Inventor 汪志勇唐林查正根
Owner UNIV OF SCI & TECH OF CHINA
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