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Preparation method of 3-methyl methoxyacrylate

A technology of methyl methoxy acrylate and methyl ethoxy propionate, which is applied in the field of preparation of methyl 3-methoxy acrylate, can solve problems such as difficult industrialization, expensive catalysts, and difficult recycling, and achieve cost low cost, simple method and ideal yield

Active Publication Date: 2013-05-22
HUNAN HAILI CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] The main product of this method is methyl 3,3-dimethoxypropionate, and the catalyst used is expensive and difficult to recycle, resulting in high cost and difficult to realize industrialization

Method used

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  • Preparation method of 3-methyl methoxyacrylate
  • Preparation method of 3-methyl methoxyacrylate
  • Preparation method of 3-methyl methoxyacrylate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 135g (833mmol) methyl 3-methoxy-3-ethoxypropionate, 800g methanol, and 2g potassium bisulfate to a 2000mL three-neck flask, heat and reflux for 24 hours after the addition, and change the reflux device to vacuum distillation device, and the solvent was removed under reduced pressure. The residue was heated to 140°C for 30 hours under the protection of nitrogen under normal pressure, and then distilled under reduced pressure to obtain 76.4 g (659 mmol) of methyl 3-methoxyacrylate with a purity of 97% (normalized by gas chromatography). The rate is 76.66%.

Embodiment 2

[0021] Add 135g (833mmol) methyl 3-methoxy-3-ethoxypropionate, 1200g methanol, and 2g sodium bisulfate to a 2000mL three-necked flask. Pressure distillation device, desolvent under reduced pressure; the residue was decompressed to 60mmHg, heated to 60°C for 10 hours, and then distilled under reduced pressure to obtain 72.2g (622mmol) of methyl 3-methoxyacrylate with a purity of 96% (gas phase Chromatographic normalization), the yield was 71.70%.

Embodiment 3

[0023] Add 100g (617mmol) methyl 3-methoxy-3-ethoxypropionate, 1500g methanol, and 5g sodium bisulfate to a 2000mL three-necked flask, heat and reflux for 48 hours after the addition, and change the reflux device to vacuum distillation equipment, and remove the solvent under reduced pressure; the residue was heated to 160°C under normal pressure for 5 hours of cracking reaction, and then distilled under reduced pressure to obtain 55.1g (475mmol) of methyl 3-methoxyacrylate with a purity of 95% (normalized by gas chromatography) , yield 73.10%.

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Abstract

The invention discloses a preparation method of 3-methyl methoxyacrylate. 3-methyl methoxyacrylate is prepared in the presence of a catalyst potassium hydrogen sulfate or sodium hydrogen sulfate by adopting 3-methoxy-3-ethyoxyl methyl propionate and methanol as raw materials; and the chemical reaction formula is shown in the formula of the description. According to the preparation method of 3-methyl methoxyacrylate, provided by the invention, 3-methoxy-3-ethyoxyl methyl propionate and methanol which are easily prepared are adopted and used as the raw materials and are synthesized in the presence of the catalyst to obtain the target product. The method is simple and convenient, easy to operate, wide in raw material source, suitable for industrial production and higher in competitiveness, and is a preparation method with low cost and ideal yield.

Description

technical field [0001] The present invention relates to the preparation of methyl 3-methoxyacrylate, which is valuable for various purposes, such as use as a pesticide or a pharmaceutical intermediate. Background technique [0002] Methyl 3-methoxyacrylate is an important pharmaceutical and pesticide intermediate, such as an intermediate for the insecticide flonicamid. According to the literature, there are mainly the following synthetic methods at home and abroad. [0003] One, take methyl propiolate as raw material, carry out addition reaction with methanol, as document Journal of Organic Chemistry, 2010,75 (22), 7809-7821 reports methyl propiolate and methanol under the effect of catalyst, with Methyl 3-methoxyacrylate was obtained in 71% yield. [0004] [0005] The method raw material methyl propiolate is expensive, resulting in higher costs. [0006] 2. Using methyl 3,3-dimethoxypropionate as a raw material, it is prepared by cracking under the action of a cataly...

Claims

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Application Information

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IPC IPC(8): C07C69/734C07C67/327
Inventor 胡志彬王晓光黄超群彭鹏罗正孙炯熊莉莉罗亮明
Owner HUNAN HAILI CHEM IND
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