CN108047172B - Method for preparing 2-methyl-5, gamma-dioxotetrahydrofuran-2-pentanoic acid by catalyzing levulinic acid - Google Patents

Method for preparing 2-methyl-5, gamma-dioxotetrahydrofuran-2-pentanoic acid by catalyzing levulinic acid Download PDF

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CN108047172B
CN108047172B CN201711292380.0A CN201711292380A CN108047172B CN 108047172 B CN108047172 B CN 108047172B CN 201711292380 A CN201711292380 A CN 201711292380A CN 108047172 B CN108047172 B CN 108047172B
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levulinic acid
dioxotetrahydrofuran
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CN108047172A (en
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邓天昇
李政
侯相林
王玉琪
王英雄
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Shanxi Institute of Coal Chemistry of CAS
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    • C07D307/02Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
    • C07D307/26Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having one double bond between ring members or between a ring member and a non-ring member
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Abstract

A process for preparing 2-methyl-5, gamma-dioxotetrahydrofuran-2-pentanoic acid by catalyzing levulinic acid includes mixing protonic acid with levulinic acid, adding catalyst, heating to 70-200 deg.C, and reacting for 0.25-96 h. Vacuum distilling, dissolving the residue with organic solvent, filtering, removing metal ion catalyst, adding excessive weak base reagent into the filtrate, filtering, and distilling the filtrate to obtain 2-methyl-5, gamma-dioxotetrahydrofuran-2-pentanoic acid. The invention has the advantages of high conversion rate of levulinic acid and high product yield.

Description

Method for preparing 2-methyl-5, gamma-dioxotetrahydrofuran-2-pentanoic acid by catalyzing levulinic acid
Technical Field
The invention relates to a method for preparing 2-methyl-5, gamma-dioxotetrahydrofuran-2-pentanoic acid by catalyzing levulinic acid.
Technical Field
Levulinic acid (4-pentanoic acid) is an important biomass-based platform compound, which is classified as the 12 most important platform compounds for saccharide conversion by the U.S. national energy agency. From the chemical structure, the levulinic acid is a five-carbon straight-chain compound containing two functional groups, namely carbonyl and carboxyl. Currently, lignocellulose can be efficiently converted to levulinic acid in a continuous industrial reactor by a biorefinery process. Whereas lignocellulose is the most abundant biomass resource in the world, the generation of the biomass-based platform compound levulinic acid has strong competitiveness (reaching 0.06-0.18 pounds at present), and has the potential to become a bulk chemical.
The catalytic conversion of levulinic acid is an important link in the utilization and conversion process of biomass at present, since levulinic acid contains a carbonyl group and a carboxyl group, various reactions such as carbonyl reduction/carboxyl esterification/ammoniation and the like can occur, and the subsequent conversion products of levulinic acid mainly comprise: levulinate, gamma-valerolactone, angelicin, 2-methyltetrahydrofuran, aminolevulinic acid and the like. Levulinic acid is a C5 small molecular compound, and in order to break through the limitation of the carbon chain number of a levulinic acid molecule on the range of downstream products, the selective breakage of C-C bonds and the generation technology of new C-C bonds form the key challenges of catalytic conversion of the levulinic acid. Since levulinic acid contains a carbonyl group with relatively stable chemical properties, the carburation technology mainly utilizes the aldol condensation reaction of the alpha-H connected with the carbonyl group and active groups of other compounds such as aldehyde carbonyl, for example: aldol condensation of levulinic acid with furfural, 5-hydroxymethylfurfural, glyoxylic acid and other compounds. However, levulinic acid contains a ketone carbonyl group, theoretically, a new carbon-carbon bond can be generated through self aldol condensation, so that a C10 compound is generated, the compound often contains 1-2 carboxyl groups, dicarboxylic acid/diol and branched alkane can be generated through selective catalytic hydrogenation, and the compounds are important fine chemicals or high molecular polymerization monomer raw materials, but the research on the self condensation reaction of the levulinic acid is less at present. Spanish scientists have invented a reaction process for catalyzing aldol condensation of levulinic acid by using alkaline metal, the reaction temperature is low, the blending is mild, but the levulinic acid is an organic acid and can react with an alkaline catalyst, the stability of the catalyst is poor, and the acidity of carboxyl is stronger than that of alpha-H on the levulinic acid, so that the alkaline catalyst is easy to react with the carboxyl, and the activity of a catalytic system is low. Shell company adopts strong acids such as molecular sieve and acidic resin as catalysts to catalyze dimerization of levulinic acid, but the products are numerous, the stability of the acidic resin in an organic phase is poor, and the pore passages of the molecular sieve are easy to block, thereby bringing great limitation to the industrial production of the acidic resin.
Disclosure of Invention
The invention aims to provide a method for preparing 2-methyl-5, gamma-dioxotetrahydrofuran-2-pentanoic acid by catalyzing conversion of levulinic acid and self-addition with high efficiency.
Levulinic acid does not readily undergo an aldol condensation reaction due to the presence of carboxyl groups. Without special pore restrictions and surface enrichment, conventional acidic catalysts are not effective in catalyzing the self-addition reaction of levulinic acid. Carboxyl in the levulinic acid is easy to react with an acidic catalytic center, so that the configuration of the levulinic acid is changed, and the catalytic activity is influenced. The acid sites of the macroporous acidic resin and the molecular sieve are mostly distributed in the catalyst pore channels, the spatial confinement effect of the pore channels can reduce the configuration transformation of the levulinic acid and inhibit the effect of carboxyl groups on the acid sites, however, the levulinic acid is an organic acid, and a large number of hydrogen bonds exist in the system, so that the viscosity of the system is high, particularly when the levulinic acid undergoes addition or polymerization reaction, the viscosity is increased more remarkably, the viscosity seriously affects the proceeding speed of catalytic reaction, and the blockage of the pore channels of the catalyst is caused, so that the catalyst is inactivated. Therefore, an efficient/economic/green catalytic conversion self-addition catalytic system for levulinic acid must have the characteristics of homogeneous phase/no action between an active center and carboxyl, and the like, and based on the consideration, the following catalytic reaction process is developed and designed.
The interaction of the carboxyl group with the catalytic central site is a key factor affecting the aldol condensation of levulinic acid. The conventional protonic acid and metal ion inevitably react with the carboxyl group on levulinic acid, thereby destroying the activity of the catalyst. Different metal cations have different L-acid properties, and the different metal cations are selected to react with carbonyl groups to catalyze the aldol condensation reaction of the levulinic acid, but do not react with carboxylic acid, so that the catalytic activity of catalyzing the aldol condensation of the levulinic acid is maintained. In addition, the B acid tends to have a concerted catalytic effect on the catalytic reaction of the L acid. Based on the method, the invention provides a method for catalyzing dimerization of levulinic acid, which is a method for selectively preparing a decacarbon compound, namely 2-methyl-5, gamma-dioxotetrahydrofuran-2-pentanoic acid (the structural formula is shown in the specification) by catalyzing the levulinic acid to perform a reaction process similar to aldol condensation by using metal cations as catalytic active centers and protonic acid as a cocatalyst.
Figure BDA0001499628070000031
The method comprises the following specific operation steps:
(1) mixing protonic acid and levulinic acid according to the mass ratio of 0.5-0.1g to 1g to prepare reaction liquid;
(2) adding a catalyst accounting for 2-30% of the mass of the levulinic acid into the prepared reaction solution to prepare a reaction system;
(3) heating the prepared reaction system to 70-200 ℃ and reacting for 0.25-96 h.
(4) Distilling under reduced pressure to remove unreacted levulinic acid, fully dissolving the residue after distillation with an organic solvent, filtering to remove the metal ion catalyst, adding an excessive weak base reagent into the filtrate, filtering, and distilling the filtrate to obtain the 2-methyl-5, gamma-dioxotetrahydrofuran-2-pentanoic acid.
The protonic acid in said (1) is a homogeneous strong acid, preferably trichloroacetic acid, hydrochloric acid, sulfuric acid, etc.
The catalyst in the step (2) is halide formed by zinc ions, copper ions, ferric ions or tetravalent tin ions.
The process conditions of reduced pressure distillation in the step (4) are that the pressure is 0.5-3KPa and the temperature is 50-150 ℃.
The organic solvent in the step (4) refers to low-carbon ketone, low-carbon ester or low-carbon ether, and the like, preferably acetone, ethyl acetate and diethyl ether, wherein the volume mass ratio of the solvent amount to the raw material levulinic acid is 10-1 ml: 1g of the total weight of the composition.
The weak base reagent in the step (4) refers to sodium carbonate, sodium bicarbonate, potassium carbonate or potassium bicarbonate,
the addition amount is 1-5 times of the amount of protonic acid substance.
Compared with the prior art, the invention has the following advantages:
1. the catalyst used in the invention is conventional metal salt, so the source is wide and the price is low.
2. The catalyst of the invention can reduce the adverse effect of carboxyl on catalyzing aldol condensation reaction.
3. The viscosity of the product is gradually increased in the reaction process, the homogeneous catalysis system reduces the adverse effect of the diffusion of substances in the high-viscosity system on the reaction, the catalytic reaction has higher yield, and finally, the conversion rate of the levulinic acid is more than 45 percent, and the yield is more than 40 percent.
Drawings
FIG. 1 is an NMR-HSQC (C-H correlation) spectrum of the product.
FIG. 2 is an NMR-C13 spectrum of the product, wherein A and B are the corresponding magnified effect plots of C.
FIG. 3 is an NMR-dept spectrum of the product.
Figure 4 is a levulinic acid MS spectrum.
Figure 5 is the MS spectrum of the product.
Detailed Description
Example 1
10g of levulinic acid and 5g of trichloroacetic acid were mixed thoroughly, and 1.36g of ZnCl2 was added to prepare a reaction solution. The reaction solution was heated to 130 ℃ and reacted for 6 hours. The structural characterization of 2-methyl-5, gamma-dioxotetrahydrofuran-2-pentanoic acid is shown in the figure (the results of NMR and MS are shown in the figures 1-5). And distilling the reaction product at 150 ℃ under reduced pressure of 3kPa until no liquid is distilled off, dissolving the distillation residue with 10ml of acetone, filtering, adding 3g of potassium bicarbonate into the filtrate, filtering, and evaporating the filtrate to dryness to obtain 4.2g of the target product, wherein the purity of the product is 95%. Levulinic acid conversion was 45% and overall process yield was 40%.
Example 2
10g of levulinic acid and 1g of concentrated hydrochloric acid are fully mixed, and then 0.2g of ZnBr2 is added to prepare reaction liquid. The reaction solution was heated to 120 ℃ and reacted for 6 hours. And distilling the reaction product at 140 ℃ under reduced pressure of 2.5kPa until no liquid is distilled off, dissolving the reaction product with 20ml of ethyl acetate, filtering, adding 1g of sodium bicarbonate into the filtrate, filtering, and evaporating the filtrate to dryness to obtain 5g of the target product, wherein the purity of the product is 89%. Levulinic acid conversion was 48% and overall process yield was 44.5%.
Example 3
10g of levulinic acid and 2g of concentrated sulfuric acid are fully mixed, and 0.5g of FeCl3 is added to prepare a reaction solution. The reaction solution was heated to 70 ℃ and reacted for 96 hours. And distilling the reaction product at 130 ℃ under reduced pressure of 2kPa until no liquid is distilled off, dissolving the reaction product by using 30ml of acetone, filtering, adding 5g of potassium carbonate into the filtrate, filtering, and evaporating the filtrate to dryness to obtain 5.1g of a target product, wherein the purity of the product is 90%. Levulinic acid conversion was 50% and overall process yield was 46%.
Example 4
1g of levulinic acid and 4g of trichloroacetic acid were mixed thoroughly, and then 0.08g of CuCl2 was added to prepare a reaction solution. The reaction solution was heated to 180 ℃ and reacted for 1 hour. And distilling the reaction product at 120 ℃ under reduced pressure of 1.5kPa until no liquid is distilled off, dissolving the reaction product with 1ml of diethyl ether, filtering, adding 13g of sodium carbonate into the filtrate, filtering, and evaporating the filtrate to dryness to obtain 0.45g of the target product, wherein the purity of the product is 92%. Levulinic acid conversion was 46% and overall process yield was 41%.
Example 5
1g levulinic acid and 2g concentrated hydrochloric acid were mixed thoroughly, and then 0.16g SnCl4 was added to prepare a reaction solution. The reaction solution was heated to 150 ℃ and reacted for 4 hours. And distilling the reaction product at 80 ℃ under reduced pressure of 1kPa until no liquid is distilled off, dissolving the reaction product by using 1ml of acetone, filtering, adding 8g of sodium carbonate into the filtrate, filtering, and evaporating the filtrate to dryness to obtain 0.51g of a target product, wherein the purity of the product is 91%. Levulinic acid conversion was 49% and overall process yield was 46%.
Example 6
1g of levulinic acid and 3g of concentrated hydrochloric acid are fully mixed, and then 0.18g of ZnBr2 is added to prepare a reaction solution. The reaction solution was heated to 190 ℃ and reacted for 0.5 h. And distilling the reaction product at 50 ℃ under reduced pressure of 0.5kPa until no liquid is distilled off, dissolving the reaction product with 1ml of ethyl acetate, filtering, adding 5g of sodium carbonate into the filtrate, filtering, and evaporating the filtrate to dryness to obtain 0.48g of the target product, wherein the purity of the product is 94%. Levulinic acid conversion was 48% and overall process yield was 45%.
Example 7
10g of levulinic acid and 4g of concentrated hydrochloric acid are fully mixed, and then 2g of ZnCl2 is added to prepare a reaction solution. The reaction solution was heated to 80 ℃ and reacted for 90 hours. And distilling the reaction product at 150 ℃ under reduced pressure of 3kPa until no liquid is distilled off, dissolving the reaction product by using 70ml of acetone, filtering, adding 15g of sodium carbonate into the filtrate, filtering, and evaporating the filtrate to dryness to obtain 5.6g of a target product, wherein the purity of the product is 88%. Levulinic acid conversion was 53% and overall process yield was 49%.
Example 8
1g of levulinic acid and 5g of concentrated hydrochloric acid are fully mixed, and then 0.25g of ZnCl2 is added to prepare a reaction solution. The reaction solution was heated to 90 ℃ and reacted for 82 hours. And distilling the reaction product at 80 ℃ under reduced pressure of 1kPa until no liquid is distilled off, dissolving the reaction product by using 1ml of acetone, filtering, adding 18g of sodium carbonate into the filtrate, filtering, and evaporating the filtrate to dryness to obtain 0.51g of a target product, wherein the purity of the product is 92%. Levulinic acid conversion was 51% and overall process yield was 47%.
Example 9
A reaction solution was prepared by thoroughly mixing 1g of levulinic acid and 2g of concentrated hydrochloric acid, and then adding 0.28g of FeCl 3. The reaction solution was heated to 100 ℃ and reacted for 20 hours. And distilling the reaction product at 100 ℃ under reduced pressure of 1kPa until no liquid is distilled off, dissolving the reaction product with 1ml of diethyl ether, filtering, adding 4g of sodium carbonate into the filtrate, then filtering, and evaporating the filtrate to dryness to obtain 0.46g of the target product, wherein the purity of the product is 93%. Levulinic acid conversion was 46% and overall process yield was 43%.
Example 10
1g of levulinic acid and 3g of concentrated hydrochloric acid are fully mixed, and then 0.3g of ZnCl2 is added to prepare a reaction solution. The reaction solution was heated to 200 ℃ and reacted for 0.25 h. And distilling the reaction product at 10 ℃ under reduced pressure of 1.5kPa until no liquid is distilled off, dissolving the reaction product with 1ml of acetone, filtering, adding 10g of sodium carbonate into the filtrate, filtering, and evaporating the filtrate to dryness to obtain 0.52g of the target product, wherein the purity of the product is 92%. Levulinic acid conversion 52% and overall process yield 48%.
Example 11
10g of levulinic acid and 4g of concentrated sulfuric acid are fully mixed, and then 0.2g of ZnCl2 is added to prepare a reaction solution. The reaction solution was heated to 110 ℃ and reacted for 6 hours. And distilling the reaction product at 130 ℃ under reduced pressure of 2kPa until no liquid is distilled off, dissolving the reaction product by using 80ml of ethyl acetate, filtering, adding 10g of sodium carbonate into the filtrate, filtering, and evaporating the filtrate to dryness to obtain 5.3g of a target product, wherein the purity of the product is 95%. Levulinic acid conversion was 55% and overall process yield was 50%.
Example 12
10g of levulinic acid and 3g of concentrated sulfuric acid are fully mixed, and then 0.8g of ZnCl2 is added to prepare a reaction solution. The reaction solution was heated to 140 ℃ and reacted for 4 hours. And distilling the reaction product at 140 ℃ under reduced pressure of 2.5kPa until no liquid is distilled off, dissolving the reaction product by using 90ml of acetone, filtering, adding 8g of sodium carbonate into the filtrate, filtering, and evaporating the filtrate to dryness to obtain 5.5g of a target product, wherein the purity of the product is 91%. Levulinic acid conversion 57% and overall process yield 50%.
Example 13
10g of levulinic acid and 2g of concentrated sulfuric acid are fully mixed, and then 0.3g of ZnCl2 is added to prepare a reaction solution. The reaction solution was heated to 140 ℃ and reacted for 3 hours. And distilling the reaction product at 130 ℃ under reduced pressure of 2kPa until no liquid is distilled off, dissolving the reaction product by using 60ml of acetone, filtering, adding 6g of sodium carbonate into the filtrate, filtering, and evaporating the filtrate to dryness to obtain 4.6g of a target product, wherein the purity of the product is 93%. Levulinic acid conversion was 48% and overall process yield was 43%.
Example 14
10g of levulinic acid and 2g of concentrated sulfuric acid are fully mixed, and then 1g of ZnCl2 is added to prepare a reaction solution. The reaction solution was heated to 160 ℃ and reacted for 2 h. And distilling the reaction product at 120 ℃ under reduced pressure of 1.5kPa until no liquid is distilled off, dissolving the reaction product with 50ml of acetone, filtering, adding 6g of sodium carbonate into the filtrate, filtering, and evaporating the filtrate to dryness to obtain 4.8g of a target product, wherein the purity of the product is 89%. Levulinic acid conversion was 45% and overall process yield was 43%.
Example 15
10g of levulinic acid and 1g of concentrated sulfuric acid are fully mixed, and 1.5g of ZnCl2 is added to prepare a reaction solution. The reaction solution was heated to 180 ℃ and reacted for 1 hour. And distilling the reaction product at 150 ℃ under reduced pressure of 3kPa until no liquid is distilled off, dissolving the reaction product by using 30ml of acetone, filtering, adding 4g of sodium carbonate into the filtrate, filtering, and evaporating the filtrate to dryness to obtain 4.6g of a target product, wherein the purity of the product is 94%. Levulinic acid conversion 47% and overall process yield 43%.
Example 16
1g of levulinic acid and 3g of concentrated sulfuric acid are fully mixed, and then 0.18g of CuBr2 is added to prepare a reaction solution. The reaction solution was heated to 110 ℃ and reacted for 6 hours. And distilling the reaction product at 150 ℃ under reduced pressure of 3kPa until no liquid is distilled off, dissolving the reaction product by using 8ml of ethyl acetate, filtering, adding 10g of sodium carbonate into the filtrate, filtering, and evaporating the filtrate to dryness to obtain 0.48g of a target product, wherein the purity of the product is 94%. Levulinic acid conversion was 49% and overall process yield was 45%.
Example 17
10g of levulinic acid and 2g of concentrated sulfuric acid are fully mixed, and then 3g of ZnCl2 is added to prepare a reaction solution. The reaction solution was heated to 130 ℃ and reacted for 6 hours. And distilling the reaction product at 150 ℃ under reduced pressure of 3kPa until no liquid is distilled off, dissolving the reaction product with 10ml of ether, filtering, adding 8g of sodium bicarbonate into the filtrate, filtering, and evaporating the filtrate to dryness to obtain 5.1g of the target product, wherein the purity of the product is 93%. Levulinic acid conversion was 52% and overall process yield was 47%.
Example 18
10g of levulinic acid and 4g of trichloroacetic acid were mixed thoroughly, and 2g of ZnCl2 was added to prepare a reaction solution. The reaction solution was heated to 140 ℃ and reacted for 4 hours. And distilling the reaction product at 130 ℃ under reduced pressure of 2kPa until no liquid is distilled off, dissolving the reaction product by using 20ml of acetone, filtering, adding 4g of sodium bicarbonate into the filtrate, filtering, and evaporating the filtrate to dryness to obtain 5.3g of a target product, wherein the purity of the product is 92%. Levulinic acid conversion was 56% and overall process yield was 49%.
Example 19
10g of levulinic acid and 4g of trichloroacetic acid were mixed thoroughly, and 2.4g of FeCl3 was added to prepare a reaction solution. The reaction solution was heated to 140 ℃ and reacted for 4 hours. And distilling the reaction product at 150 ℃ under reduced pressure of 3kPa until no liquid is distilled off, dissolving the reaction product by using 30ml of acetone, filtering, adding 4g of sodium bicarbonate into the filtrate, filtering, and evaporating the filtrate to dryness to obtain 5.4g of a target product, wherein the purity of the product is 88%. Levulinic acid conversion was 56% and overall process yield was 48%.
Example 20
10g of levulinic acid and 4g of trichloroacetic acid were mixed thoroughly, and 2.8g of ZnCl2 was added to prepare a reaction solution. The reaction solution was heated to 140 ℃ and reacted for 3 hours. The reaction product was distilled at 150 ℃ under reduced pressure of 3kPa until no liquid distilled, dissolved in 10ml of ethyl acetate, filtered, and 8g of sodium bicarbonate was added to the filtrate, followed by filtration, and the filtrate was evaporated to dryness to give 5.3g of the desired product, the purity of the product being 93%. Levulinic acid conversion 58% and overall process yield 49%.
Example 21
10g of levulinic acid and 4g of trichloroacetic acid were mixed thoroughly, and 3g of ZnCl2 was added to prepare a reaction solution. The reaction solution was heated to 140 ℃ and reacted for 3 hours. And distilling the reaction product at 150 ℃ under reduced pressure of 3kPa until no liquid is distilled off, dissolving the reaction product with 50ml of ether, filtering, adding 10g of sodium bicarbonate into the filtrate, filtering, and evaporating the filtrate to dryness to obtain 5.2g of the target product, wherein the purity of the product is 91%. Levulinic acid conversion was 55% and overall process yield was 47%.
Example 22
10g of levulinic acid and 4g of trichloroacetic acid were mixed thoroughly, and 1.5g of SnCl4 was added to prepare a reaction solution. The reaction solution was heated to 140 ℃ and reacted for 2 hours. And distilling the reaction product at 140 ℃ under reduced pressure of 3kPa until no liquid is distilled off, dissolving the reaction product by using 80ml of acetone, filtering, adding 10g of sodium bicarbonate into the filtrate, filtering, and evaporating the filtrate to dryness to obtain 5.4g of a target product, wherein the purity of the product is 92%. Levulinic acid conversion 57% and overall process yield 49%.
Example 23
10g of levulinic acid and 4g of trichloroacetic acid were mixed thoroughly, and 1.5g of ZnCl2 was added to prepare a reaction solution. The reaction solution was heated to 140 ℃ and reacted for 3 hours. And distilling the reaction product at 150 ℃ under reduced pressure of 3kPa until no liquid is distilled out, dissolving the reaction product by using 60ml of ethyl acetate, filtering, adding 5g of potassium bicarbonate into the filtrate, filtering, and evaporating the filtrate to dryness to obtain 5.3g of a target product, wherein the purity of the product is 92%. Levulinic acid conversion was 56% and overall process yield was 49%.
Example 24
10g of levulinic acid and 4g of trichloroacetic acid were mixed thoroughly, and 1.8g of ZnCl2 was added to prepare a reaction solution. The reaction solution was heated to 140 ℃ and reacted for 2 hours. And distilling the reaction product at 150 ℃ under reduced pressure of 3kPa until no liquid is distilled off, dissolving the reaction product with 10ml of ether, filtering, adding 4g of sodium bicarbonate into the filtrate, filtering, and evaporating the filtrate to dryness to obtain 5.4g of the target product, wherein the purity of the product is 94%. Levulinic acid conversion was 56% and overall process yield was 50%.

Claims (7)

1. A method for preparing 2-methyl-5, gamma-dioxotetrahydrofuran-2-pentanoic acid by catalyzing levulinic acid, is characterized by comprising the following steps: the method comprises the following steps:
(1) mixing protonic acid and levulinic acid according to the mass ratio of 0.5-0.1g to 1g to prepare a reaction solution, wherein the protonic acid is trichloroacetic acid, hydrochloric acid or sulfuric acid;
(2) adding a catalyst accounting for 2-30% of the mass percent of the levulinic acid into the prepared reaction solution to prepare a reaction system, wherein the catalyst is a halide formed by zinc ions, copper ions, ferric ions or tetravalent tin ions;
(3) heating the prepared reaction system to 70-200 ℃ and reacting for 0.25-96 h;
(4) distilling under reduced pressure to remove unreacted levulinic acid, fully dissolving the residue after distillation with an organic solvent, filtering to remove the metal ion catalyst, adding an excessive weak base reagent into the filtrate, filtering, and distilling the filtrate to obtain the 2-methyl-5, gamma-dioxotetrahydrofuran-2-pentanoic acid.
2. The method of claim 1, wherein the levulinic acid is catalyzed to produce 2-methyl-5, γ -dioxotetrahydrofuran-2-pentanoic acid: the process conditions of reduced pressure distillation in the step (4) are that the pressure is 0.5-3KPa and the temperature is 50-150 ℃.
3. The method of claim 1, wherein the levulinic acid is catalyzed to produce 2-methyl-5, γ -dioxotetrahydrofuran-2-pentanoic acid: the organic solvent in the step (4) is one of low-carbon ketone, low-carbon ester or low-carbon ether.
4. The method of claim 1, wherein the levulinic acid is catalyzed to produce 2-methyl-5, γ -dioxotetrahydrofuran-2-pentanoic acid: the organic solvent in the step (4) is one of acetone, ethyl acetate or diethyl ether.
5. The method of claim 1, wherein the levulinic acid is catalyzed to produce 2-methyl-5, γ -dioxotetrahydrofuran-2-pentanoic acid: the volume mass ratio of the organic solvent dosage in the step (4) to the raw material levulinic acid is 10-1 ml: 1g of the total weight of the composition.
6. The method of claim 1, wherein the levulinic acid is catalyzed to produce 2-methyl-5, γ -dioxotetrahydrofuran-2-pentanoic acid: the weak base reagent in the step (4) is one of sodium carbonate, sodium bicarbonate, potassium carbonate or potassium bicarbonate.
7. The method of claim 1, wherein the levulinic acid is catalyzed to produce 2-methyl-5, γ -dioxotetrahydrofuran-2-pentanoic acid: the addition amount of the weak base reagent in the step (4) is 1-5 times of the amount of the protonic acid substance.
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