Method for synthesizing 2,5-dimethylamino furan through catalytic hydrogenation of 2,5-diformaldehyde oxime furan
A technology of dimethylaminofuran and dimethylaminofuran, which is applied in the field of catalytic hydrogenation of 2,5-dimethylaminofuran to synthesize 2,5-dimethylaminofuran, can solve the problem of poor safety and reusability, catalyst Solve the problems of large dosage and low catalytic activity, and achieve the effect of easy separation, high catalytic activity and good product selectivity
Active Publication Date: 2018-06-08
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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Problems solved by technology
The above research shows that metals such as Raney Ni can catalyze the hydrogenation of 2,5-dimethylaldoxime furan to synthesize 2,5-dimethylaminofuran, but the problem is that the catalytic activity is low and the amount of catalyst used is large
In addition, due to the poor stability of Raney Ni in the air, there are also problems of poor safety and reusability in use.
Method used
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[0019] Example: Add 1 mmol of 2,5-dimethylaldoxime furan, 30 mg of Rh / HZSM-5 catalyst with a loading capacity of 5 wt%, and 7 mL of methanol into a 15 mL reactor, and replace the air in the reactor with hydrogen for 10 times. After raising the temperature to 130°C, fill it with hydrogen to 2MPa, and start stirring. If the partial pressure of hydrogen drops, make up to 2MPa. After 3 hours of reaction, it was cooled to room temperature. The reaction solution was centrifuged to separate the catalyst, and samples were taken, and liquid chromatography was used for product analysis. Such as figure 1 Shown is the high-performance liquid chromatography (HPLC) diagram of the reaction solution, in which the retention time is 8.136min is the raw material 2,5-dimethylaldoxime furan, and the retention time is 15.251min is the product 2,5-dimethylaminofuran . A small amount of by-products are partially dehydrated products, and there are also diamine and triamine compounds containing mul...
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The invention discloses a method for synthesizing 2,5-dimethylamino furan through catalytic hydrogenation of 2,5-diformaldehyde oxime furan. According to the method, mesoporous and microporous molecular sieve supported active metal components are taken as a catalyst, and 2,5-diformaldehyde oxime furan is hydrogenated, dehydrated and converted into 2,5-dimethylamino furan in a high-selectivity manner. The reaction system uses mild reaction conditions and is simple to operate; the prepared product 2,5-dimethylamino furan has high purity; the used multi-phase catalyst is simple to prepare, high in activity and selectivity and easy to separate from the system and can be repeatedly used.
Description
technical field [0001] The invention relates to a method for synthesizing 2,5-dimethylaminofuran by catalytic hydrogenation of 2,5-dimethylaldoxime furan. In the method, active metal components supported by mesoporous and microporous molecular sieves are used as catalysts, and 2, Hydrodehydration of 5-dimethylaldoxime furan to 2,5-dimethylaminofuran with high selectivity. Background technique [0002] 2,5-Dimethylaminofuran is an important class of chemical raw materials and intermediates, and has important applications in the fields of medicine, dyes, and pesticides. 2,5-Dimethylaminofuran has the characteristics of a polymer monomer, and can synthesize new polyurethane and polyamide polymer materials through polymerization. Therefore, the development of a synthetic route for 2,5-dimethylaminofuran has great application value. [0003] In recent years, studies have shown that metals such as Raney Ni can be used to catalyze the hydrogenation of 2,5-dimethylaldoxime furan t...
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Login to View More IPC IPC(8): C07D307/52
CPCC07D307/52
Inventor 徐杰徐永明马继平高进苗虹李晓芳
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI