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Application of a Nitrogen-Containing Ordered Mesoporous Carbon Catalyst in the Synthesis of Higher β-Ketoesters by Transesterification

A catalyst and mesoporous carbon technology, which is applied in the field of catalyzing the transesterification of simple β-ketoesters and alcohols to prepare advanced β-ketoesters, which can solve the problems of poor stability, low catalytic activity, and high price

Active Publication Date: 2019-03-22
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The technical problem to be solved in the present invention is to provide a catalyst with high catalytic activity and high product yield for the problems of low catalytic activity, high price, poor stability, and metal pollution of the catalysts currently used for the transesterification reaction of β-ketone esters and alcohols. , a new type of catalyst that is easy to separate after the reaction and can be reused

Method used

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  • Application of a Nitrogen-Containing Ordered Mesoporous Carbon Catalyst in the Synthesis of Higher β-Ketoesters by Transesterification

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] (1) Add 30 molar parts of ethyl acetoacetate, 10 molar parts of butanol, and 4 molar parts of catalyst into a flask, and react at 110° C. for 6 h.

[0021] (2) Centrifuge the catalyst after completion of the reaction. The product was analyzed by gas chromatography, and the yield of the target product butyl acetoacetate was 97%.

Embodiment 2

[0023] (1) Add 30 molar parts of ethyl acetoacetate, 10 molar parts of butanol, and 4 molar parts of catalyst into a flask, and react at 110° C. for 4 hours.

[0024] (2) Centrifuge the catalyst after completion of the reaction. The product was analyzed by gas chromatography, and the yield of the target product butyl acetoacetate was 90%.

Embodiment 3

[0026] (1) Add 25 molar parts of ethyl acetoacetate, 10 molar parts of butanol, and 3 molar parts of catalyst into a flask, and react at 100° C. for 6 h.

[0027] (2) Centrifuge the catalyst after completion of the reaction. The product was analyzed by gas chromatography, and the yield of the target product butyl acetoacetate was 85%.

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Abstract

The invention relates to a reaction for synthesizing higher beta-ketoester by adopting NOMC (nitrogen-doped ordered mesoporous carbon) as a heterogeneous catalyst for catalyzing transesterification between simple beta-ketoester and alcohol. According to the reaction, NOMC is taken as the catalyst, beta-ketoester and alcohol are taken as the raw materials, the reaction is performed at the temperature of 90-110 DEG C for 4-6 h, and the highest yield of higher beta-ketoester can reach 97%. Compared with the conventional commonly-used homogeneous catalyst for the catalytic reaction, the reaction has the advantages that the catalyst is convenient to recover, the product is convenient to separate and the like.

Description

technical field [0001] The invention belongs to the field of heterogeneous catalysis, and specifically relates to a method for preparing high-grade β-ketoesters by using nitrogen-containing ordered mesoporous carbon as a catalyst to catalyze the transesterification reaction of simple β-ketoesters and alcohols. Background technique [0002] β-ketoester is an important intermediate in chemical production. β-ketoesters can be used as raw materials to synthesize biochemical reagents such as thiolactomycin, prostaglandin, and syncarpic acid. Transesterification is a general synthesis method for β-ketoesters, that is, simple β-ketoesters (such as ethyl formoacetate and ethyl acetoacetate) are transesterified with higher alcohols to synthesize higher β-ketoesters and lower alcohols . The reaction equation is shown in the figure below, where R 1 = H, CH 3 ; 2 =CH 3 , C 2 h 5 ; 3 ≥C 2 h 5 . [0003] [0004] Since the transesterification reaction of β-ketoesters and al...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/72C07C67/03B01J27/24
CPCB01J27/24C07C67/03C07C69/72
Inventor 许杰马丹薛冰柳娜李永昕
Owner CHANGZHOU UNIV