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A kind of method for preparing amide compound

A technology of amide compounds and amine compounds, which is applied in the field of preparation of amide compounds, can solve the problems of easy deactivation of catalysts, difficulty in separation, complex preparation of ligands, etc., and achieve good product applicability, simple preparation, and good selectivity Effect

Active Publication Date: 2022-03-08
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Although the current method of preparing amides has made some progress, there are still problems, such as long preparation routes, tedious preparation of catalysts, complex preparation of ligands, the need for co-catalysts, difficulty in separation, and easy deactivation of catalysts.

Method used

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  • A kind of method for preparing amide compound
  • A kind of method for preparing amide compound
  • A kind of method for preparing amide compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] In a 15 mL Teflon-lined reactor, add 2 mL THF, 0.3 mmol styrene, 0.5 mmol benzylamine and 0.1 g of 0.15 wt% Ru / CeO 2 Catalyst, add magneton, fill with 0.5MPa CO, airtight, stir and react at 180°C for 12h, after the reaction, the product is qualitative by mass spectrogram and quantitative by gas chromatography. The conversion rate and selectivity of styrene are shown in Table 1. The product looks like this:

[0044]

[0045]The product 1 is a direct chain product, and the product 2 is a branched chain product.

Embodiment 2

[0047] In a 15mL Teflon-lined reactor, add 2mL THF, 0.5mmol aniline, and 0.1g of 2wt% Ru / CeO 2 Catalyst, add magnetons, fill with 0.5MPa ethylene, 0.5MPa CO, airtight, stir and react at 180°C for 4h, after the reaction, the product is qualitative by mass spectrogram and quantitative by gas chromatography. The conversion rate and selectivity of aniline are shown in Table 1. The product looks like this:

[0048]

Embodiment 3

[0050] In a 15mL Teflon-lined reactor, add 2mL THF, 0.5mmol aniline, and 0.1g of 5wt% Ru / CeO 2 Catalyst, add magnetons, fill with 0.5MPa ethylene, 0.5MPa CO, airtight, stir and react at 180°C for 4h, after the reaction, the product is qualitative by mass spectrogram and quantitative by gas chromatography. The conversion rate and product selectivity of aniline are shown in Table 1. Product is with embodiment 1.

[0051]

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PUM

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Abstract

The invention relates to a method for preparing amide compounds. The method adopts amines, olefins and carbon monoxide as reaction substrates, organic solvents as solvents, and prepares amide compounds under the catalysis of ruthenium-supported metal oxides. The reaction process is as follows: Add solvent, amine, olefin and catalyst into the pressure vessel, fill it with carbon monoxide, seal it, stir, the reaction temperature is not lower than 130°C, and the reaction time is not less than 2 hours. After the reaction, the catalyst and the reaction system are easy to separate And it can be recycled for many times, and the yield of amide compounds can reach up to 90%.

Description

technical field [0001] The invention relates to a method for preparing amide compounds, in particular to the preparation of amide compounds by hydroamidation reaction of olefin, carbon monoxide and amine. Background technique [0002] Amide compounds and derivatives of amide compounds have important uses in medicine, chemical industry, fuel, etc., such as synthesizing perfumes, flavoring agents, detergents, and surfactants. [0003] Methods for the preparation of amides have been reported. In 2013, Matthias Beller's research group reported an article using homogeneous Pd as a catalyst, p-benzenemethanesulfonic acid as an acid additive, and adding phosphorus ligands. The pressure of CO required in the reaction is 3MPa, to Preparation of amides (Fang, X.; Jackstell, R.; Beller, M. Angew. Chem. Int. Ed, 2013, 52, 14089.). In 2015, Professor Huang Hanmin of the State Key Laboratory of Oxidative Synthesis and Selective Oxidation, Lanzhou Institute of Chemistry, Chinese Academy ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C231/10C07C233/11C07C233/07C07C233/58C07C233/06B01J23/46B01J23/63B01J23/64
CPCC07C231/10B01J23/462B01J23/63B01J23/6484C07C2601/14C07C233/11C07C233/07C07C233/58C07C233/06
Inventor 王峰安静华王业红张志鑫张健
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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