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Synthesis method of 5-methyl-2-pyrrolidone

A pyrrolidone and synthesis method technology, applied in chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, organic chemistry, etc., can solve the problem of large amount of Raney nickel catalyst, unstable skeleton structure, and reduced catalyst activity and other issues, to achieve the effect of improving safety and environmental protection, high selectivity, and simple operation

Inactive Publication Date: 2019-12-27
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the amount of Raney nickel catalyst is relatively large (20mg / mmol levulinic acid), and the skeleton structure is unstable, and it is easy to be crushed during the reaction process, resulting in a reduction in catalyst activity.

Method used

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  • Synthesis method of 5-methyl-2-pyrrolidone
  • Synthesis method of 5-methyl-2-pyrrolidone
  • Synthesis method of 5-methyl-2-pyrrolidone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Get 0.5g levulinic acid and 0.27g ammonium formate in the beaker, add 10mL water, dissolve, add the solution in the 25mL autoclave, add the Pd-Ni / C catalyst (Pd, Ni of The mass ratio is 1:1), purging five times with nitrogen gas, and reacting for 3 hours at a reaction temperature of 120°C to obtain 5-methyl-2-pyrrolidone with a yield of 65.6%.

Embodiment 2

[0036]Get 0.5g levulinic acid and 1g ammonium formate in the beaker, add 10mL water, dissolve, solution is added in the 25mL autoclave, add the Pd-Ni / C catalyst (the mass of Pd, Ni of 0.05g loading capacity of 5wt%) The ratio is 1:1), purging five times with nitrogen gas, and reacting for 3 hours at a reaction temperature of 180°C to obtain 5-methyl-2-pyrrolidone with a yield of 94.5%.

Embodiment 3-5

[0038] Other operations are the same as in Example 2, changing the type of supported bimetallic catalyst (the metal loading is 5wt%, and the mass ratio of bimetal is 1:1), to obtain the following reaction results (Table 1):

[0039] Table 1

[0040]

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Abstract

The invention discloses a preparation method of 5-methyl-2-pyrrolidone. A biomass derivative levulinic acid is used as an initial raw material; ammonium formate is used as a hydrogen source and a nitrogen source; a supported bimetallic catalyst is used as a hydrogenation catalyst; and the 5-methyl-2-pyrrolidone is synthesized in water by adopting a one-pot method. The supporting metal of the supported bimetallic catalyst is bimetallic composed of two precious metals, bimetallic composed of one precious metal and one non-precious metal A or non-precious metal B, or bimetallic composed of one non-precious metal A and one non-precious metal B. According to the method, the conversion rate of the levulinic acid can reach 100%, and the yield of the 5-methyl-2-pyrrolidone can reach 94% or above.The method provided by the invention has the advantages of environment-friendly process, simple operation, recyclable catalyst, high reaction selectivity, high product yield, and obvious industrial production advantages.

Description

technical field [0001] The invention relates to a preparation method of 5-methyl-2-pyrrolidone, in particular to a method for preparing 5-methyl-2-pyrrolidone by catalytic reductive amination of levulinic acid and ammonium formate under the action of a supported bimetallic catalyst. Background technique [0002] With the depletion of non-renewable fossil resources such as coal, oil and natural gas, research on the production of high value-added chemicals and fuels using typical renewable resource biomass as a substitute has attracted more and more attention. Effective transformation of biomass renewable resources can reduce dependence on fossil energy, alleviate current resource and energy problems in my country and the world, and achieve sustainable development. Biomass can be converted into bulk platform compounds and biofuels such as 5-hydroxymethylfurfural, γ-valerolactone, levulinic acid, and N-substituted alkylpyrrolidones. [0003] 5-Methyl-2-pyrrolidone is an import...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D207/267B01J23/89B01J23/889B01J23/656B01J23/755
CPCB01J23/6567B01J23/755B01J23/8892B01J23/8896B01J23/892C07D207/267Y02P20/584
Inventor 刘迎新王鋆史潇洋魏作君
Owner ZHEJIANG UNIV OF TECH
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