Preparation method for methyl methoxyacetate

A technology for methyl methoxyacetate and methyl acetate, applied in the field of preparing methyl methoxyacetate, can solve the problems of large equipment investment, serious pollution, unsuitability for industrialization, etc., and achieves high yield and low equipment corrosion. , the effect of mild reaction conditions

Inactive Publication Date: 2012-09-26
XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The yield and selectivity of the carbonylation reaction are relatively low, which is not suitable for industrialization; the yield of methyl methoxyacetate generated by the esterification reaction of chloroacetic acid and sodium methylate is relatively low; the reaction energy consumption of ethylene glycol monomethyl ether is large, Serious pollution, large investment in equipment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] a. In a stainless steel autoclave with a volume of 200ml, add 35.2g (0.46mol) of raw material methylal, 46.0g (1.0mol) of formic acid, and then add 0.4g of catalyst p-toluenesulfonic acid, close the reactor, and the reaction temperature is 120 ℃, the reaction time is 6 hours, and the pressure of the reaction system is 1MPa;

[0019] b. After the reaction, the reactor was cooled to room temperature, and the feed liquid in the reactor was taken out, and analyzed by gas chromatography, the yield of methyl methoxyacetate was 85%.

Embodiment 2

[0021] a. In a stainless steel autoclave with a volume of 200ml, add 44.0g (0.58mol) of raw material methylal, 66.0g (1.43mol) of formic acid, and then add 1.80g of catalyst cation exchange resin, the reaction temperature is 100°C, and the reaction time is 6 hour, the pressure of the reaction system is 2MPa;

[0022] b. After the reaction, the reactor was cooled to room temperature, and the feed liquid in the reactor was taken out, and analyzed by gas chromatography, the yield of methyl methoxyacetate was 35%.

Embodiment 3

[0024] a. In a stainless steel autoclave with a volume of 200ml, add 17.5g (0.23mol) of raw material methylal, 23.0g (0.50mol) of formic acid, and then add 0.48g of catalyst cation exchange resin, the reaction temperature is 120°C, and the reaction time is 4 hour, the pressure of the reaction system is 1.5MPa;

[0025] b. After the reaction, the reactor was cooled to room temperature, and the liquid in the reactor was taken out, and analyzed by gas chromatography, the yield of methyl methoxyacetate was 47%.

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PUM

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Abstract

The invention relates to a preparation method for methyl methoxyacetate. The preparation method for methyl methoxyacetate includes steps of taking methylal and formic acid as raw materials, adding a catalyst, and synthesizing the methyl glycolate under quite low temperature and quite low pressure. The preparation method for methyl methoxyacetate is low in catalyst corrosion to reaction equipment and mild in reaction conditions. The selectivity of methyl methoxyacetate obtained by the preparation method can be up to over 90 %,and the yield coefficient can be up to over 86%.

Description

technical field [0001] The invention relates to a method for preparing methyl methoxyacetate by using methylal and formic acid as raw materials under the action of a catalyst. Background technique [0002] Methyl methoxyacetate is an important organic chemical raw material, which is widely used in the dynamic resolution of chiral amine compounds, the synthesis of vitamin B6 and sulfa-5-pyrimidine, and the catalyst for polymerization reactions; in addition, it is the production Intermediates of ethylene glycol. [0003] There are three main methods for the synthesis of methyl methoxyacetate: 1) using methanol or methylal dimethanol as raw materials to synthesize through carbonylation; 2) using chloroacetic acid and sodium methylate as raw materials to first synthesize methoxyacetic acid , the latter synthesizes methyl methoxyacetate through esterification reaction with methanol; 3) takes ethylene glycol monomethyl ether as raw material, synthesizes methoxyacetic acid through...

Claims

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Application Information

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IPC IPC(8): C07C69/708C07C67/24
Inventor 吾满江・艾力沈鑫权高志贤刘洪忠
Owner XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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