Method for preparing 2, 5-dimethylamino furan from 2, 5-diformyl furan

A technology of diformylfuran and dimethylaminofuran, which is applied in the field of preparation of 2,5-dimethylaminofuran to achieve the effects of less by-products, simple catalyst system and high product quality

Active Publication Date: 2015-01-14
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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After careful review of the literature, as far

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0020] Example 1: Add 1mmol of 2,5-diformylfuran and 0.002mmol of Ni / CaO catalyst with a loading capacity of 5wt% to a 15mL reaction kettle, add 2mL of acetonitrile, close the kettle, replace the air in the kettle with hydrogen for 10 times, and flush Hydrogen, the partial pressure is 0.5MPa, and then filled with ammonia, the partial pressure is 0.5MPa, then stirred at 25°C for 0.5h, heated to 80°C, and kept for 3h. After the reaction, the reacted mixture was cooled to room temperature, and the catalyst was removed by centrifugation. Samples were taken and analyzed by gas chromatography. The conversion rate of raw materials was 99%, and the selectivity was 99%. The solvent was removed by distillation, the solid was washed with saturated brine, and filtered to obtain a white solid. Dry in vacuo to give a white solid. The product purity reaches more than 99%. The isolated yield was 98%.

Embodiment 2

[0021] Example 2: 10-fold magnification experiment: Add 10mmol of 5-hydroxymethylfurfural and 0.02mmol of 5wt%Ni / CaO catalyst into a 50mL reaction kettle, add 20mL of acetonitrile, close the kettle, and replace the air in the kettle with hydrogen for 10 times , into hydrogen, the partial pressure is 0.5MPa, then filled with ammonia, the partial pressure is 0.5MPa, then stirred at 25°C for 5h, heated to 80°C, and kept for 30h. After the reaction, according to the method described in Example 1, the reacted mixture was cooled to room temperature for sampling analysis. The raw material conversion rate is 99%, and the selectivity is 99%. The isolated yield was 97%.

Embodiment 3

[0022] Example 3: Add 1mmol of 2,5-diformylfuran and 0.001mmol of a 1wt% Pt / MgO catalyst into a 15mL reaction kettle, add 2mL of ethanol, close the kettle, replace the air in the kettle with hydrogen for 10 times, and flush Hydrogen, the partial pressure is 0.4MPa, then filled with ammonia, the partial pressure is 0.6MPa, then stirred at 25°C for 1h, heated to 100°C, and kept for 4h. After the reaction, according to the method described in Example 1, cooling and sampling analysis, the conversion rate of raw materials is greater than 99%, and the selectivity is greater than 99%. The isolated yield was 95%.

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Abstract

The invention discloses a method for preparing 2, 5-dimethylamino furan by catalytic reductive amination of 2, 5-diformyl furan, according the method, ammonia is used as an amine source, hydrogen is used as a hydrogen source, a loading type metal is used as a catalyst, and the 2, 5-dimethylamino furan is prepared by selective reductive amination of the 2, 5-diformyl furan at 30-220 DEG C. The method has the advantages that reaction conditions are mild, product yield is high, the catalyst is easy to separate and recycle, and the product is easy to separate and purify, the purity of the product reaches more than 99%, and the product has a 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-diformyl furan. Specifically, it uses a supported metal catalyst system, using ammonia as the amine source, hydrogen as the hydrogen source, and under mild conditions, the reductive amination of 2,5-diformylfuran to prepare 2,5-dimethylamino furan. Background technique [0002] It has an important scientific background and application to efficiently convert renewable biomass resources into energy chemicals and polymer monomers to replace or supplement the shortage of fossil resources such as petroleum, and to alleviate the pressure on the environment caused by petroleum-based polymers that are difficult to degrade. prospect. 5-Hydroxymethylfurfural is widely regarded as one of the important biomass-based platform compounds, which can be prepared by acid-catalyzed dehydration of carbohydrates, such as fructose, glucose, sucrose, cellulos...

Claims

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Application Information

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IPC IPC(8): C07D307/52B01J23/755B01J23/42B01J23/835B01J23/34B01J23/52B01J23/46B01J23/68B01J23/63B01J23/648B01J23/28B01J23/89B01J23/14B01J23/26
CPCY02P20/584C07D307/52B01J23/14B01J23/26B01J23/28B01J23/34B01J23/36B01J23/42B01J23/462B01J23/52B01J23/63B01J23/6484B01J23/682B01J23/745B01J23/78B01J23/835B01J23/8906
Inventor 马继平徐杰贾秀全王敏石松苗虹高进
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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