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A kind of method for preparing ester compound

A compound and oxide technology, applied in the field of preparation of ester compounds, can solve problems such as difficult separation, easy deactivation of catalysts, complex preparation of ligands, etc., and achieve the effects of high catalyst activity, good product applicability, and good selectivity

Active Publication Date: 2020-01-07
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 ester compounds has made some progress, there are still problems, such as long preparation routes, low yield of target products, cumbersome preparation of catalysts, complex preparation of ligands, need for co-catalysts, and difficult separation and catalysts. Vulnerable to deactivation and other issues

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] In a 50mL Teflon-lined reactor, add 4mL of methanol, 0.3mmol of styrene, and 0.1g of 0.15wt% 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 50 mL Teflon-lined reactor, add 4 mL of ethanol, 0.1 mmol of styrene, and 0.1 g of 0.15 wt% Ru / TiO 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:

[0048]

[0049] The product 1 is a direct chain product, and the product 2 is a branched chain product.

Embodiment 3

[0051] In a 50mL Teflon-lined reactor, add 4mL methanol, 0.5mmol styrene, and 0.1g of 5wt% 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. Product is with embodiment 1.

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Abstract

The invention relates to an ester-based compound preparation method, which comprises: adding an alcohol-based compound, an olefin and a ruthenium-loaded metal oxide catalyst to a pressure container, wherein the alcohol-based compound is used as a solvent and a raw material; inflating with carbon monoxide; sealing; and stirring, wherein the reaction temperature is more than or equal to 130 DEG C, the reaction time is more than or equal to 2 h, the ruthenium-loaded metal oxide catalyst is one or a plurality of materials selected from Ru / TiO2, Ru / Nb2O5, Ru / CeO2 and Ru / Al2O3, and the mass fractionof ruthenium in the ruthenium-loaded metal oxide catalyst is 0.15-10 wt%. According to the present invention, after the reaction, the catalyst is easily separated from the reaction system, and can berecycled a plurality of times; and the yield of the ester-based compound can be up to 86%.

Description

technical field [0001] The invention relates to a method for preparing ester compounds, in particular to the preparation of ester compounds by alkoxy carbonylation reaction of olefin, carbon monoxide and alcohol. Background technique [0002] Esters and derivatives of esters have important uses in medicine, chemicals, fuels, etc., such as synthetic perfumes, flavoring agents, detergents, and surfactants. [0003] Methods for the preparation of ester compounds have been reported. Howard Alper et al. (Organic Letters, 2006, 8, 6143.) used palladium acetate as the main catalyst, boric acid esters generated in situ from boric acid and salicylic acid as catalysts, and added phosphine monodentate ligands to synthesize Anti-Mark rule linear esters. Pedro A.Aguirre et al. (Dalton Trans, 2007, 5419.) used Pd metal complexes containing N and P ligands as catalysts, and p-benzenemethanesulfonic acid (TsOH) as acid co-catalysts to catalyze the methoxylation of alkenes Carbonylation r...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/36C07C69/612C07C69/24C07C69/75C07C69/14
CPCC07C67/36C07C69/612C07C69/24C07C69/75C07C69/14
Inventor 王峰安静华王业红张志鑫张健侯婷婷张晓辰
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI