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Synthesis method of methyl 3-methoxypropionate

A technology for the synthesis of methyl methoxypropionate, which is applied in the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of organic compounds, and can solve the problems of catalysts being unable to be reused, reaction equipment corroded, and high preparation costs. To achieve the effect of short reaction time, avoid corrosion and fast reaction speed

Pending Publication Date: 2021-12-07
JIANGSU HUALUN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the problem that the catalyst in the existing preparation method of methyl 3-methoxypropionate cannot be reused and the existing preparation technology needs to add acid to neutralize the catalyst, which leads to the corrosion of the reaction instrument, resulting in high preparation cost, Problems such as waste of resources and waste treatment are caused, the present invention provides a new synthetic method of methyl 3-methoxypropionate, the synthetic method of the present invention overcomes the above-mentioned defects, and brings significant economic and environmental benefits. benefit

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A kind of synthetic method of 3-methoxy propionate methyl ester, comprises following concrete steps:

[0027] (1) First build the reaction device: the three-necked flask is respectively equipped with a condenser (connected to the drier), a thermometer and a constant pressure dropping funnel, and puts a stirring bar of a moderate size, and uses a magnetic oil bath to heat and provide stirring power; 2.47mol (79.0g) of methyl alcohol and 0.00013mol (0.03g) of methyltributylammonium chloride (quaternary ammonium salt ionic liquid catalyst) join in the anti-there three-necked flask, then adopt the mode of dropping to pass through the constant pressure dropping funnel Add 1.23mol (106.2g) of methyl acrylate dropwise into the three-necked flask, and heat to 38°C for addition reaction, control the methyl acrylate for 1.5 hours to complete the dropwise addition, and continue the reaction for 1 hour after the dropwise addition;

[0028] (2) After the reaction, the unreacted raw ...

Embodiment 2

[0031] A kind of synthetic method of 3-methoxy propionate methyl ester, comprises following concrete steps:

[0032] (1) First build the reaction device: the three-necked flask is respectively equipped with a condenser (connected to the drier), a thermometer and a constant pressure dropping funnel, and puts a stirring bar of a moderate size, and uses a magnetic oil bath to heat and provide stirring power; 2.47mol (79.0g) of methyl alcohol and 0.00014mol (0.02g) of tetraethylammonium hydroxide (quaternary ammonium salt ionic liquid catalyst) join in the anti-three-necked flask, then adopt the mode of dropping to pass through the constant pressure dropping funnel to three-necked Add 0.99 mol (84.9 g) of methyl acrylate dropwise into the flask, and heat to 40°C for addition reaction, control methyl acrylate for 1 hour to complete the dropwise addition, and continue the reaction for 1.5 hours after the dropwise addition;

[0033] (2) After the reaction, the unreacted raw material ...

Embodiment 3

[0036] A kind of synthetic method of 3-methoxy propionate methyl ester, comprises following concrete steps:

[0037] (1) First build the reaction device: the three-necked flask is respectively equipped with a condenser (connected to the drier), a thermometer and a constant pressure dropping funnel, and puts a stirring bar of a moderate size, and uses a magnetic oil bath to heat and provide stirring power; 2.47mol (79.0g) of methanol and 0.00016mol (0.08g) of tributyl (2-methoxyethyl) phosphorus bis (trifluoromethylsulfonyl) imide (quaternary ammonium salt ionic liquid catalyst) is added to the reverse three port In the flask, then dropwise add 0.82mol (70.8g) of methyl acrylate into the three-necked flask through the constant pressure dropping funnel by means of dropwise addition, and heat to 43°C for addition reaction, and control the methyl acrylate for 1 hour to complete All are added dropwise, and the reaction is continued for 1 hour after the dropwise addition is complete...

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Abstract

The invention discloses a synthesis method of methyl 3-methoxypropionate, which comprises the steps of carrying out addition reaction at low temperature by taking methanol and methyl acrylate as raw materials and quaternary ammonium salt ionic liquid as a catalyst, distilling and collecting unreacted raw materials after the reaction is completed, and then carrying out reduced pressure distillation to obtain a methyl 3-methoxypropionate product. Methanol and methyl acrylate serve as the raw materials, the quaternary ammonium salt ionic liquid serves as the catalyst, and methyl 3-methoxypropionate is synthesized under the low-temperature condition. After the reaction is completed, acid does not need to be added to neutralize the catalyst, so that the problem of corrosion of neutralized acid to a reaction container is avoided, and meanwhile, the preparation cost is also reduced; and according to the synthesis process disclosed by the invention, unreacted raw materials can be directly distilled and collected under normal pressure, and then reduced pressure distillation is performed to obtain the methyl 3-methoxypropionate product, the residue after reduced pressure distillation is the quaternary ammonium salt ionic liquid catalyst, and the catalyst can be repeatedly recycled, so that the cost is reduced, and the resource waste is reduced.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a method for synthesizing methyl 3-methoxypropionate. Background technique [0002] Methyl 3-methoxypropionate is a colorless liquid with a special odor, with a boiling point of 142°C-143°C, non-toxic to humans, and moderate volatility. It is an important environment-friendly solvent and organic synthesis intermediate, widely used in electronics industry, cleaning industry, paint industry, pesticide industry and organic synthesis and other fields. [0003] According to the existing literature reports, the main synthetic method of methyl 3-methoxypropionate is: methyl acrylate is slowly added dropwise in excess methanol, and under low temperature conditions, it is decomposed by alkali metal salts such as sodium methylate and potassium methylate. Under the influence of addition reaction to generate 3-methoxy propionate methyl ester pre-product, then add acid to neutrali...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/31C07C69/708B01J31/02
CPCC07C67/31B01J31/0281B01J2231/32C07C69/708Y02P20/584
Inventor 吴昊戴鑫任倩李茉潘学林
Owner JIANGSU HUALUN CHEM