Preparation method of dimethyl fumarate

A technology for dimethyl fumarate and dimethyl fumarate is applied in the field of preparation of catalyzed synthesis of dimethyl fumarate, and can solve the problems of complicated post-processing operations, difficult recovery of catalysts, and equipment corrosion. and other problems, to achieve the effect of stable product quality, environmental improvement, and reduction of equipment corrosion.

Inactive Publication Date: 2009-07-08
SHANGHAI CHEM REAGENT RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The technical problem that the present invention solves is to provide a kind of preparation method of dimethyl fumarate (DMF), to overcome the shortcomi...

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  • Preparation method of dimethyl fumarate
  • Preparation method of dimethyl fumarate

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Embodiment 1

[0020] In a reactor equipped with heating, stirring, thermometer, and reflux condensing device, 125ml of methanol, 49g (0.5mol) of maleic anhydride and 2.5g of solid acid SO were added at room temperature. 4 2- / Al 2 o 3 Catalyst, while stirring, gradually heat up to reflux, control the reaction temperature at 60°C, react for 5.0 hours, cool the reaction solution to room temperature, filter, dissolve the precipitate with ethyl acetate, filter to remove solid acid SO 4 2- / Al 2 o 3 Catalyst (can be recycled after recovery), the ethyl acetate layer is washed with 100ml 8wt% NaOH solution, the separated ethyl acetate layer is washed with water to neutrality, and the solvent ethyl acetate is evaporated (recovered and reused) to obtain a white solid The product dimethyl fumarate was 62.91 g, and the yield was 87.34%. Melting point: 103.1-103.5°C. Purity: 98.7% (HPLC).

Embodiment 2

[0022] In a reactor equipped with heating, stirring, thermometer, and reflux condensing device, add 150ml of methanol, 49g (0.5mol) of maleic anhydride and 5g of solid acid SO at room temperature. 4 2- / Al 2 o 3 Catalyst, gradually heat up to reflux while stirring, control the reaction temperature at 65°C, cool to room temperature after 10 hours of reaction, filter, dissolve the precipitate with ethyl acetate, filter to remove solid acid SO 4 2- / Al 2 o 3 Catalyst (recycling after recovery), ethyl acetate layer uses 125ml 9wt%Na 2 CO 3 The solution was washed, and the separated ethyl acetate layer was washed with water until neutral, and the solvent ethyl acetate was evaporated (recovered and reused) to obtain 64.88 g of dimethyl fumarate as a white solid product, with a yield of 90.11%. Melting point: 102.9-103.3°C. Purity: 97.9% (HPLC).

Embodiment 3

[0024] In a reactor equipped with heating, stirring, thermometer, and reflux condensing device, 175ml of methanol, 49g (0.5mol) of maleic anhydride and 8g of solid acid SO were added at room temperature. 4 2- / Al 2 o 3 Catalyst, the reaction temperature is controlled at 70 °C, after 8 hours of reaction, cool to room temperature, filter, dissolve the precipitate with ethyl acetate, and filter to remove solid acid SO 4 2- / Al 2 o 3 Catalyst (recycling after recovery), ethyl acetate layer uses 140ml 10wt%NaHCO 3 The solution was washed, and the separated ethyl acetate layer was washed with water until neutral, and the solvent was evaporated (recovered and reused) to obtain 66.97 g of dimethyl fumarate as a white solid product, with a yield of 93.01%. Melting point: 102.8-103.1°C. Purity: 98.2% (HPLC).

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Abstract

The invention discloses a method for preparing fumaric dimethyl ester (DMF). The method comprises the steps of taking maleic anhydride as raw material and subjecting the raw material and methanol to catalytic reaction in the presence of a solid-acid SO4/Al2O3 catalyst so as to obtain the fumaric dimethyl ester, namely a target product of the invention. The purity of the fumaric dimethyl ester obtained by the preparation method is up to over 98.5 percent, and the yield of the fumaric dimethyl ester is between 85 and 95 percent. Compared with the prior art, the method has the advantages that the method adopts the solid-acid SO4/Al2O3 catalyst, is safe and convenient in operation, improves environment, reduces corrosion on equipment, can cyclically recycle reaction solvent and the solid-acid catalyst, reduces the three wastes, ensures stable product quality, and is suitable for industrial production.

Description

technical field [0001] The present invention relates to the preparation method of dimethyl fumarate, more specifically, relate to a kind of preparation method of catalytic synthesis dimethyl fumarate. Background technique [0002] Dimethyl fumarate (DMF) is an important new high-efficiency preservative, which has broad-spectrum high-efficiency, bacteriostasis, bactericidal effect, and insecticidal effect. It is low in price and good in chemical stability. A low-toxic, safe food additive. After DMF enters the human body, it can quickly transform into fumaric acid and become a normal metabolic component in the human body. Its structural formula is as follows: [0003] [0004] Existing many patents and literature have reported the preparation method of DMF at present, as reported in the Chinese patent CN 86106666 take maleic anhydride and methyl alcohol as raw material, react under the presence of concentrated hydrochloric acid, prepare DMF; Chemical World, 1994( 4): 190-...

Claims

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Application Information

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IPC IPC(8): C07C69/657C07C67/08B01J27/02B01J21/04
CPCY02P20/584
Inventor 顾慧娟周重道廖本仁
Owner SHANGHAI CHEM REAGENT RES INST
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