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Method of preparing methyl furoate

A technology for methyl furoate and furfural, applied in the field of preparing methyl furoate, can solve the problems of difficult recovery of homogeneous alkali, high price of precious metals and the like, and achieve the effects of low cost, low price and mild reaction conditions

Inactive Publication Date: 2019-04-05
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the problems of high price of precious metals and difficult recovery of homogeneous alkali still need to be solved

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 1mmol of furfural, 250mmol of methanol, 0.15mmol of N-hydroxyphthalimide and 5mL of 30% hydrogen peroxide aqueous solution into a 50mL round-bottomed flask, stir and react at room temperature and pressure for 16h, and the liquid obtained after the reaction The mixture was separated, and the liquid phase product containing methyl furoate was taken for detection. After gas chromatography analysis, the yield of methyl furoate was 20.6%.

Embodiment 2

[0024] Add 1mmol of furfural, 231mmol of methanol, 0.12mmol of N-hydroxyphthalimide and 4mL of 30% hydrogen peroxide aqueous solution into a 50mL round bottom flask, stir and react at room temperature and pressure for 19h, and the liquid obtained after the reaction The mixture was separated, and the liquid phase product containing methyl furoate was taken for detection. After gas chromatography analysis, the yield of methyl furoate was 34.5%.

Embodiment 3

[0026] Add 1mmol of furfural, 210mmol of methanol, 0.059mmol of N-hydroxyphthalimide and 4mL of 30% hydrogen peroxide aqueous solution into a 50mL round-bottom flask, stir and react at room temperature and pressure for 18h, and the liquid obtained after the reaction The mixture was separated, and the liquid phase product containing methyl furoate was taken for detection. After gas chromatography analysis, the yield of methyl furoate was 38.6%.

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Abstract

The invention discloses a method of preparing methyl furoate. methyl furoate is prepared by catalyzing one-step oxidative esterification of furfural through a homogenous catalyst. The method includesthe steps of dissolving furfural in methanol, adding a catalyst and an oxidant, and stirring under room temperature to normal pressure to allow reacting; after reacting, subjecting the product to liquid-liquid separation, and collecting the liquid-phase product methyl furoate. The method allows methyl furoate to be prepared by one-step oxidative esterification through furfural and methanol; the method is simple to perform, low in cost, easy to separate and green.

Description

technical field [0001] The invention relates to a method for preparing methyl furoate, which belongs to the technical field of energy and chemical industry. Background technique [0002] Methyl furoate is an important new synthetic fragrance, which can be widely used in food, beverage and cosmetic industries as a flavor modifier and flavor enhancer, and has been approved for use by the United States. [0003] At present, the method of artificially synthesizing methyl furoate is mainly to use the oxidation product of furfural, furoic acid, to carry out the esterification reaction with methanol. In comparison, the one-step oxidative esterification of furfural and methanol to prepare methyl furoate has more advantages. At present, there are relatively few reports on the oxidative esterification of furfural to methyl furoate, and there are mainly two types of catalytic systems: non-noble metal Co-N-C catalysis and noble metal catalysis. For example, with Co-N-C as catalyst, ad...

Claims

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Application Information

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IPC IPC(8): C07D307/68
CPCC07D307/68
Inventor 曾宪海高哲邦冯云超李孟渚孙勇唐兴林鹿
Owner XIAMEN UNIV