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Synthesis method of 5-methyl-2-pyrrolidone or derivatives thereof

A pyrrolidone and synthetic method technology, applied in the field of organic catalytic synthesis, can solve the problems of product separation and purification difficulties, solvent volatilization and recovery, low product selectivity, etc., and achieve the effect of facilitating separation, avoiding side reactions, and simple reaction system

Active Publication Date: 2019-10-01
XIAMEN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] The purpose of the present invention is to overcome the deficiencies of the prior art, and provides a synthetic method of 5-methyl-2-pyrrolidone or its derivatives, which solves the problem of high hydrogen pressure and a large amount of organic matter caused by the external hydrogen source in the above-mentioned background technology. The problem of solvent volatilization and recovery caused by solvent use also solves the problems of low product selectivity and difficulty in product separation and purification

Method used

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  • Synthesis method of 5-methyl-2-pyrrolidone or derivatives thereof
  • Synthesis method of 5-methyl-2-pyrrolidone or derivatives thereof
  • Synthesis method of 5-methyl-2-pyrrolidone or derivatives thereof

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Experimental program
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Effect test

Embodiment 1～6

[0031] Take 0.05mol of levulinic acid, methyl levulinate, ethyl levulinate, propyl levulinate, butyl levulinate, amyl levulinate respectively, and put them in high pressure reaction with equimolar urea and formic acid In the still, add 0.174g ruthenium carbon catalyst and mix evenly, seal the reaction kettle, heat to 130°C under magnetic stirring and keep for 6h respectively, finish the reaction and cool to room temperature and filter to recover the catalyst. GC-MS (Shimadzu) and GC (Agilent) were used for qualitative and quantitative detection, and the detection results are listed in Table 1 with serial numbers 1-6.

Embodiment 7～16

[0033] Take 0.1mol formamide, acetamide, propionamide, benzamide, phenylacetamide, N-methylformamide, N-methylacetamide, N-methylpropionamide, N-methylbenzamide respectively , N-methylphenylacetamide, put 0.05mol ethyl levulinate and 0.1mol formic acid in a high-pressure reactor, then add 0.29g platinum carbon catalyst and mix evenly, seal the reactor, heat to 100°C under magnetic stirring and Respectively keep 24h, finish the reaction and cool to room temperature and filter to recover the catalyst. GC-MS (Shimadzu) and GC (Agilent) were used for qualitative and quantitative detection, and the detection results are listed in Table 1 with serial numbers 7-16.

Embodiment 17～25

[0035] Take 0.05mol levulinic acid, 0.06mol formic acid, and 0.075mol urea in a high-pressure reactor, and then add 0.58g of rhodium carbon, palladium carbon, ruthenium carbon / copper oxide, platinum carbon / copper oxide, rhodium carbon / copper oxide , palladium carbon / copper oxide, platinum / molybdenum oxide, platinum / titanium dioxide, and platinum / zirconia catalysts were mixed evenly, and the reaction vessel was sealed, heated to 80°C under magnetic stirring and kept for 4 hours respectively. After the reaction was completed, the reaction was cooled to room temperature and the catalyst was recovered by filtration. GC-MS (Shimadzu) and GC (Agilent) were used for qualitative and quantitative detection, and the detection results are listed in Table 1 with serial numbers 17-25.

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Abstract

The invention discloses a synthesis method of 5-methyl-2-pyrrolidone or derivatives thereof, the synthesis method comprises the following steps: fully mixing levulinic acid (ester) with urea or amideand formic acid, and adding the mixture and a catalyst into a high-pressure reaction kettle for reaction to obtain the target product 5-methyl-2-pyrrolidone or derivatives thereof. After the reactionis completed, the catalyst is filtered and recovered, cleaned and dried before reuse. The method can realize efficient conversion of the levulinic acid (ester) in a solvent-free system, the low-cost and environment-friendly urea or amide is taken as a N source, and the biomass formic acid is taken as a H source, so that the synthesis method has good economy.

Description

technical field [0001] The invention belongs to the technical field of organic catalytic synthesis, and in particular relates to a synthesis method of 5-methyl-2-pyrrolidone or derivatives thereof. Background technique [0002] Pyrrolidone compounds are an important class of industrial chemicals and fine intermediates. In addition to being widely used as solvents, they can also be used in petrochemical processing, polymer synthesis, agricultural and pharmaceutical intermediates, surfactants for inks and coatings, and industrial cleaning agents. and dispersants, as well as in the manufacture of graphene and lithium-ion batteries. However, some pyrrolidone compounds, such as N-methylpyrrolidone, inevitably have toxicity and high cost in the production process, as well as increasingly stringent regulations, forcing people to seek safer and cheaper pyrrolidone compounds to replace N-methylpyrrolidone Used as a solvent. Among them, 5-methyl-2-pyrrolidone and its derivatives hav...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D207/267
CPCC07D207/267Y02P20/584
Inventor 林鹿唐兴孙勇曾宪海雷廷宙曹雪娟
Owner XIAMEN UNIV
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