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Method for preparing 2,5-dimethylaminofuran from 2,5-dimethylolfuran

A technology for dimethylolfuran and dimethylaminofuran, which is applied in the field of preparing 2,5-dimethylaminofuran, can solve problems such as complicated processes, achieves less catalyst dosage, simple catalyst system and less by-products Effect

Active Publication Date: 2016-04-13
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

The process of reductive amination of 2,5-dimethylaminofuran to prepare 2,5-dimethylaminofuran involves three steps: dehydrogenation, oxidation, amination, and hydrogenation reduction. The process is complicated. After careful literature research, according to our As far as we know, there is no report on this

Method used

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  • Method for preparing 2,5-dimethylaminofuran from 2,5-dimethylolfuran
  • Method for preparing 2,5-dimethylaminofuran from 2,5-dimethylolfuran
  • Method for preparing 2,5-dimethylaminofuran from 2,5-dimethylolfuran

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Example 1: Add 1 g of the dried carrier to the prepared HAuCl 4 4H 2 O aqueous solution (50ml, 1×10 - 3 M; calculated as Au, the load is 1wt%); stirred at 25 °C for 2 h, washed with deionized water, dried under vacuum at 25 °C for 12 h, and washed with H at 300 °C 2 Activation for 3h.

Embodiment 2

[0023] Embodiment 2: the preparation of catalyst adopts the method in embodiment 1 to carry out, only changes the solute composition in the aqueous solution, the metal source of auxiliary agent Cu, Cr, Co, Sn, Ce, Zn, Ru, Ir, Au, Ag, Pd Respectively: Cu(NO 3 ) 2 ·6H 2 O, Cr(NO 3 ) 3 9H 2 O, Co(NO 3 ) 2 ·6H 2 O, SnCl 4 ·5H 2 O, Ce(NO 3 ) 3 ·6H 2 O, Zn(NO 3 ) 2 ·6H 2 O, RuCl 3 ·3H 2 O, H 2 IrCl 6 ·6H 2 O, HAuCl 4 4H 2 O, AgNO 3 , PdCl 2 ,. Just change the molar ratio of different metal components and different supports, see Table 1 for details.

[0024]

[0025]

Embodiment 3

[0026] Example 3: Add 1mmol of 2,5-dimethylolfuran and a certain amount of supported catalyst into a 15mL reaction kettle, add 2mL of solvent, close the kettle, replace the air in the kettle with nitrogen for 10 times, and flush ammonia gas to Set the pressure, raise the temperature to the set temperature, and keep it for the set time, stir quickly, and start the reaction. After the reaction was over, the stirring was stopped, the reacted mixture was cooled to room temperature, the ammonia gas was evacuated, and samples were taken for analysis. The qualitative analysis of the product was carried out by gas chromatography-mass spectrometry and nuclear magnetic resonance spectroscopy, and the quantitative analysis was realized by gas chromatography. The purification and separation steps of the product are as follows: removing the catalyst by centrifugation, distilling off the solvent under reduced pressure, washing the solid with saturated brine, and filtering to obtain a white ...

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Abstract

The invention discloses a method for preparing 2,5-dimethylaminofuran from 2,5-dihydroxymethylfuran. The method comprises: employing ammonia gas as an amine source, taking in-situ generated active hydrogen as a hydrogen source, taking a supported metal as a catalyst, at 30-220 DEG C, performing selective reduction amination on 2,5-dihydroxymethylfuran to obtain 2,5-dimethylaminofuran. The method is mild in reaction conditions, high in product yield, and easy for separation and cycled usage of the catalyst, and also the product is easy to separate and purify, and has the purity up to 99% or more. The method has extremely good application prospect.

Description

technical field [0001] The invention relates to a method for preparing 2,5-dimethylaminofuran through catalytic reduction amination of 2,5-dimethylolfuran. Specifically, it uses a supported catalyst system, uses ammonia as the amine source, and uses the active hydrogen generated in situ as the hydrogen source to prepare 2,5-dimethylolfuran by reductive amination under mild conditions. 5-Dimethylaminofuran. Background technique [0002] Use catalytic technology to efficiently convert renewable biomass resources into energy chemicals and polymer monomers to alleviate the pressure on the environment caused by the shortage of fossil resources such as petroleum and the difficulty of degradation of petroleum-based polymers. It has important scientific background and application prospect. 2,5-Dihydroxymethylfuran is an important biomass-based monomer, which can be prepared by reducing the biomass-based platform compound 5-hydroxymethylfurfural (Chinese patent CN201210436809.X), a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/52
CPCC07D307/52
Inventor 马继平徐杰贾秀全王敏郑玺高进苗虹
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI