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Magnetically-recoverable GO/Fe3O4-CuI catalyst and preparation method and application thereof

A technology of fe3o4-cui and catalyst, which is applied in the direction of organic chemistry, can solve the problems of difficult recovery of catalyst, high catalytic efficiency, and single nature of copper salt active center, and achieve effective catalytic performance, high-efficiency catalytic performance and simple preparation

Inactive Publication Date: 2016-02-03
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there are many methods for synthesizing quinazolinone compounds. Among them, the related reports of using cuprous salt or divalent copper salt as the catalyst for the synthesis reaction of this type of compound have become more popular in recent years. The properties of the active center of copper salt as a homogeneous catalyst are compared. Single, high catalytic efficiency, less side reactions, and the mechanism of catalytic reaction is generally relatively simple, but despite this, there are still many problems in the use and industrialization of homogeneous catalysts, among which the difficult recovery of catalysts is the current scientific field. big problem

Method used

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  • Magnetically-recoverable GO/Fe3O4-CuI catalyst and preparation method and application thereof
  • Magnetically-recoverable GO/Fe3O4-CuI catalyst and preparation method and application thereof
  • Magnetically-recoverable GO/Fe3O4-CuI catalyst and preparation method and application thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Magnetic GO / Fe 3 o 4 - Preparation of CuI catalyst

[0040] (1) 1 g of graphene oxide powder is added in 300 ml of 2-pyrrolidone, and ultrasonicated for 4 hours under a nitrogen atmosphere;

[0041] (2) After ultrasonication, heat the mixture in step (1) to 190°C, and add dropwise a 2-pyrrolidone solution with a concentration of 0.1mol / L iron triacetylacetonate under mechanical stirring to make Fe 3+ The feed ratio with graphene oxide is 20mmol: 1g, stirred and refluxed for 10h;

[0042] (3) The black precipitate GO / Fe after the reaction in step (2) 3 o 4 Magnetic recovery, washed several times with absolute ethanol, vacuum dried at 45°C;

[0043] (4) The dried GO / Fe 3 o 4 Add CuI to absolute ethanol at a mass ratio of 2:1, and magnetically stir and reflux at 80°C for 8 hours under a nitrogen atmosphere. The black solid GO / Fe 3 o 4 - Magnetic recovery of CuI, washed several times with absolute ethanol, and vacuum dried at 45°C, the obtained GO / Fe 3 o 4 -CuI c...

Embodiment 2

[0049] The catalyst GO / Fe that makes in embodiment 1 3 o 4 -CuI catalyzes 2-iodobenzamide and valine to synthesize quinazolinone compounds, and the specific steps are:

[0050] (a) 0.006gGO / Fe 3 o 4 -CuI, 0.9mmol valine, 0.9mmol cesium carbonate, 0.3mmol 2-iodobenzamide and 3ml ethylene glycol / dimethyl sulfoxide were added to a 50ml round bottom flask, in ethylene glycol / dimethyl sulfoxide, ethylene di The volume ratio of alcohol to dimethyl sulfoxide is 1:60, mixed and stirred at 120°C for reflux reaction for 7 hours;

[0051] (b) The mixed solution after the reaction was recovered by magnetic adsorption to obtain a black solid, and after washing and drying, the recovered GO / Fe 3 o 4 - CuI catalyst;

[0052] (c) Extract the remaining mixed solution after magnetic recovery in step (b) with ethyl acetate / water (volume ratio is 1:1), and separate the organic phase with column chromatography to obtain quinazolinone compounds, the structural formula of the product for:

[...

Embodiment 3

[0058] The catalyst GO / Fe that makes in embodiment 1 3 o 4 -CuI catalyzes 2-iodobenzamide and norvaline to synthesize quinazolinone compounds, and the specific steps are:

[0059] (a) 0.006gGO / Fe 3 o 4 -CuI, 0.9mmol norvaline, 0.9mmol cesium carbonate, 0.3mmol 2-iodobenzamide and 3ml ethylene glycol / dimethyl sulfoxide were added to a 50ml round bottom flask, in ethylene glycol / dimethyl sulfoxide, B The volume ratio of diol and dimethyl sulfoxide is 1:60, mixed and stirred at 120°C for reflux reaction for 7 hours;

[0060] (b) Magnetically recover the mixed solution after reaction to obtain a black solid, and then wash and dry to obtain recovered GO / Fe 3 o 4 - CuI catalyst;

[0061] (c) Extract the remaining mixed solution after magnetic recovery in step (b) with ethyl acetate / water (1:1 by volume), and separate the organic phase with column chromatography to obtain quinazolinone compounds, whose structural formula is :

[0062]

[0063] The productive rate of the sy...

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Abstract

The invention relates to a magnetically-recoverable GO / Fe3O4-CuI catalyst and a preparation method and application thereof. The amount of supported Cu + in the GO / Fe3O4-CuI catalyst is 10-11% by weight, the GO / Fe3O4-CuI catalyst is prepared by adding graphene oxide powder into 2-pyrrolidone, then adding a ferric triacetylacetonate solution after ultrasonic processing, performing stirring and reflux reaction to produce a black precipitate GO / Fe3O4, adding the black precipitate and CuI into anhydrous ethanol and performing magnetic stirring reflux, the prepared GO / Fe3O4-CuI catalyst can be used for catalytic reaction of o-halogen benzamide and amino acid to generate a quinazolinone compound. Compared with the prior art, the catalyst is simple in preparation, high in catalytic activity and high in recovery rate, and the high catalytic performance of the recovered catalyst is still kept.

Description

technical field [0001] The invention belongs to the field of industrial catalysis and organic compound synthesis, and relates to the application of a novel magnetic catalyst, in particular to a magnetically recyclable GO / Fe 3 o 4 -CuI catalyst, its preparation method and the application of the catalyst in catalytic synthesis of quinazolinone compounds. Background technique [0002] Quinazolinones widely exist in natural products as skeleton structures. For example, Luotonin exists in Artemisia camelus, 2-melthyl-4(3H)-quinazolinone exists in Bacillus cereus, 2-(4-hydroxybutyl)-quinazolin-4-one exists in herb Changshan, Bouchardatine exists in rue Quinazolinone compounds in the family plants have biological activity and medicinal value, such as they can be used in hypnotics, sedatives, analgesics, antitussives, anti-inflammatory drugs, antibacterial drugs, anti-tumor drugs, anti-diabetic drugs and Anticonvulsants etc. In addition, drugs with quinazolinone as the backbone ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/122C07D239/90C07D239/91
Inventor 孔璐璐范丽岩
Owner TONGJI UNIV
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