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Preparation method of methyl 3-methoxyacrylate

A technology of methyl methoxyacrylate and methyl formate, which is applied in the field of preparation of methyl 3-methoxyacrylate, can solve the problems of unfavorable industrial production, difficulty in direct recycling, and high cost of raw materials, so as to facilitate the industrial production process , The reaction process is safe and controllable, and the effect of low raw material cost

Inactive Publication Date: 2020-05-15
ZHEJIANG BENLI TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] 3) 3,3-dimethoxypropionate methyl ester is synthesized by carbon tetrachloride and vinyl ethyl ether, this method needs to use a large amount of methanol, and produces a large amount of methanol, ethanol mixture that is difficult to directly recycle, causes raw material cost Too high, not conducive to industrial production
[0007] In summary, in the prior art, the processes using methanol and methyl acrylate as starting materials and carbon tetrachloride and vinyl ether as starting materials all have deficiencies to a certain extent, and it is necessary to develop a synthetic route that is more suitable for industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0031] The preparation method of the ionic liquid is: mix 1,3-propane sultone and methyl acetate, slowly add N-methylimidazole dropwise at 60°C for reaction, after the reaction is completed, wash and dry with methyl acetate to obtain 1- Methyl-3-(propyl 3-sulfonic acid) imidazolium salt, then take an appropriate amount of 1-methyl-3-(propyl 3-sulfonic acid) imidazolium salt dissolved in deionized water, slowly add equimolar Hydrochloric acid, reacted at 90°C for 2 hours, dehydrated under reduced pressure, dehydrated, and then cleaned the water with ethanol to obtain 1-methyl-3-(propyl-3-sulfonic acid) imidazolium chloride salt ([HO 3 S(CH 2 ) 3 -mim] Cl). Using methyl acetate as a solvent has good solubility to 1,3-propane sultone, good reaction effect, low boiling point and easy solvent removal after complete reaction; 1-methyl-3-(propyl 3-sulfonic acid) imidazole and hydrogen chloride Salt formation, if there is water, the quality of the obtained chlorine salt is poor, so...

Embodiment 1

[0035] Take 27g of sodium methoxide and place it in 200g of xylene solution, raise the temperature to 60°C, protect it with nitrogen, add dropwise 0.5mol of methyl acetate, and dropwise add a mixture of 0.58mol of methyl formate and 62g of xylene, and control the drop for 2 hours. After the addition was complete, the mixture was then kept at this temperature for 2 hours to obtain a xylene mixture of the adduct.

[0036] Add the xylene mixture of the adduct into the four-necked flask, cool down to 0-5°C, and neutralize with 15% hydrochloric acid to pH 3 under the protection of nitrogen. Stand for stratification, separate the lower water layer, add methanol 60g, ionic liquid [HO 3 S(CH 2 ) 3 -mim]Cl.AlCl 3 10g, stirred for 30min, slowly heated up to 60°C, and kept at this temperature for 3 hours. After the acetal reaction was completed, the unreacted methanol was distilled off under reduced pressure to obtain a xylene solution of the condensate.

[0037] The obtained conden...

Embodiment 2

[0039] Take 27g of sodium methoxide and place it in 200g of xylene solution, raise the temperature to 60°C, protect it with nitrogen, add dropwise 0.5mol of methyl acetate, and dropwise add a mixture of 1mol of methyl formate and 62g of xylene, and control the dropwise addition for 2 hours Finished, and then kept at this temperature for 2 hours to obtain the xylene mixture of the adduct.

[0040] Add the xylene mixture of the adduct into the four-necked flask, cool down to 0-5°C, and neutralize with 15% hydrochloric acid to pH 3 under the protection of nitrogen. Stand for stratification, separate the lower water layer, add methanol 60g, ionic liquid [HO 3 S(CH 2 ) 3 -mim]Cl.AlCl 3 10 g, stirred for 30 minutes, slowly raised the temperature to 65°C, and kept at this temperature for 3 hours. After the acetal reaction was completed, the unreacted methanol was distilled off under reduced pressure to obtain a xylene solution of the condensate.

[0041] The obtained condensate ...

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Abstract

The invention discloses a preparation method of methyl 3-methoxyacrylate. The preparation method comprises the steps: taking saturated monocarboxylic ester as a raw material and saturated carboxylic ester as an auxiliary material, and introducing formyl by utilizing methyl formate under the action of a catalyst; carrying out aldol condensation reaction with methanol under the condition that the ionic liquid is used as a catalyst, to obtain methyl 3,3-dimethoxypropionate; after the reaction is completed, separating methanol under reduced pressure, after separation is completed, increasing the temperature to 80-150 DEG C, carrying out an elimination reaction to remove one molecule of methanol on methyl 3,3-dimethoxypropionate, and thus obtaining methyl 3-methoxyacrylate, wherein methyl formate can be replaced with CO, and the raw material cost is lower. The method has the advantages of simple operation, easily available raw materials, high conversion rate, safety, environmental protection and low cost, and can realize industrial production.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a preparation method of methyl 3-methoxyacrylate. Background technique [0002] Methyl 3-methoxyacrylate is an important pharmaceutical and chemical intermediate, which can be used to synthesize a variety of organic compounds, such as cefbutan, the insecticide flonicamid, the herbicide fenpyrazone, etc. , pesticides, polymer materials and lithium batteries have broad application prospects, and the market demand is increasingly strong. [0003] The synthetic method of 3-methoxymethyl acrylate mainly contains following several kinds at present: [0004] 1) Take methyl acrylate and methanol as raw materials, and use palladium chloride and cuprous chloride as catalysts to synthesize products under high pressure. In this method, the catalyst is expensive and not easy to recycle, and the utilization rate of the catalyst is low, resulting in high cost, and the accumulation ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/734C07C67/03
CPCC07C67/03C07C69/734
Inventor 邓泉吴政杰顾海宁徐洪顺
Owner ZHEJIANG BENLI TECH CO LTD
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