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Method for preparing methyl 4-methoxy valerate from gamma-valerolactone

A technology of methyl methoxyvalerate and valerolactone, which is applied in the preparation of ester group and hydroxyl reaction, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problem of lack of material yield, properties and uses attention and other issues to achieve the effect of large application potential and good economy

Active Publication Date: 2015-02-11
XIAMEN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The literature shows that when the pentenoates are synthesized, a small amount (5% to 15%) of the by-product 4-alkoxypentenoate is usually generated (DOI: 10.1039 / c2ra23043g), but due to the lack of effective promotion The method of production of this substance, its properties and uses have not been paid attention to

Method used

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  • Method for preparing methyl 4-methoxy valerate from gamma-valerolactone
  • Method for preparing methyl 4-methoxy valerate from gamma-valerolactone
  • Method for preparing methyl 4-methoxy valerate from gamma-valerolactone

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Embodiment 1

[0018] Add 0.5g hydrogen-exchanged ultra-stable Y-type molecular sieve and 0.05g CaCO to the mixture of 10mL γ-valerolactone and 20mL methanol 3 As a catalyst, it was reacted at 250°C under a hydrogen atmosphere for 4 hours, and then filtered under reduced pressure to obtain a colorless transparent liquid. At this time, the conversion rate of γ-valerolactone was 63%, the selectivity to methyl 4-methoxyvalerate was 81%, and the selectivity to pent(en) esters was 12%.

Embodiment 2

[0020] Add 0.5g hydrogen-exchanged ultra-stable Y-type molecular sieve and 0.1g CaCO to the mixture of 5mL γ-valerolactone and 25mL methanol 3 As a catalyst, it was reacted at 250°C under a hydrogen atmosphere for 4 hours, and then filtered under reduced pressure to obtain a colorless transparent liquid. Now the gamma-valerolactone conversion rate is 65%, and the selectivity to methyl 4-methoxyvalerate is 92%, and the selectivity to pent(en) esters is 8% (such as figure 1 ).

Embodiment 3

[0022] Add 0.5g hydrogen-exchanged ultra-stable Y-type molecular sieve and 0.05g CaCO to the mixture of 10mL γ-valerolactone and 20mL methanol 3 As a catalyst, it was reacted at 250°C under a hydrogen atmosphere for 1 h, and then filtered under reduced pressure to obtain a colorless transparent liquid. At this time, the conversion rate of γ-valerolactone was 39%, the selectivity to methyl 4-methoxyvalerate was 77%, and the selectivity to pent(en) esters was 23%.

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Abstract

The invention discloses a method for preparing methyl 4-methoxy valerate from gamma-valerolactone and relates to methyl 4-methoxy valerate. The invention provides a low-cost and environment-friendly method for preparing methyl 4-methoxy valerate from gamma-valerolactone. The method comprises the following steps: (1) adding a hydrogen-exchange ultrastable Y-type molecular sieve and CaCO3 as catalysts into a mixed solution of gamma-valerolactone and methanol and reacting under an inert gas atmosphere to obtain a solid-liquid mixture; and (2) carrying out reduced pressure suction filtration on the solid-liquid mixture obtained in the step (1) to obtain a mixed solution and carrying out reduced pressure distillation on the obtained mixed solution to obtain methyl 4-methoxy valerate. Methyl 4-methoxy valerate is synthesized in a high yield from gamma-valerolactone and methanol by synergetic catalysis of the hydrogen-exchange ultrastable Y-type molecular sieve and CaCO3 for the first time and the method provides an entirely new way to biomass synthesis of high value-added chemicals.

Description

technical field [0001] The invention relates to methyl 4-methoxyvalerate, in particular to a method for preparing methyl 4-methoxyvalerate from gamma-valerolactone. Background technique [0002] γ-valerolactone (γ-valerolactone, GVL) is a new type of biomass-based platform compound synthesized from lignocellulose via levulinic acid and its esters. In recent years, due to its high calorific value, good solubility and reactivity, it has received extensive attention and research. At the same time, people have also synthesized downstream chemicals based on GVL, such as valerate or pentenoate (DOI: 10.1039 / C4CY00504J, DOI: 10.1039 / c3gc40927a, DOI: 10.1039 / c3ra23034a), butene (DOI: 10.1021 / la101424a, DOI: 10.1126 / science.1184362), 5-nonanone and derivative hydrocarbons (DOI: 10.1039 / C001899F), etc. Wherein, the main synthetic approach of preparing valeric acid esters and pentenoic acid esters by GVL is as follows: [0003] [0004] The literature shows that when the penteno...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/03C07C69/708C07C69/533B01J29/08
CPCC07C67/03B01J27/232B01J29/084B01J35/19C07C69/708C07C69/533
Inventor 曾宪海李铮蒋叶涛孙勇林鹿
Owner XIAMEN UNIV
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