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Preparation method of methyl 3-methoxyacrylate

A technology of methyl methoxyacrylate and methyl dimethoxypropionate, applied in the field of chemistry, can solve the problems of low yield, complex preparation process and high cost of methyl 3-methoxyacrylate, and achieve high yield High, less reaction steps, cost-saving effect

Pending Publication Date: 2022-01-07
昂吉(上海)环保新材料科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The object of the present invention is to solve the problems that the existing 3-methoxymethyl acrylate preparation process is complicated, the cost is high and the yield is low

Method used

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  • Preparation method of methyl 3-methoxyacrylate

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Effect test

Embodiment 1

[0035] Refer to attached figure 1 , a kind of preparation method of methyl 3-methoxyacrylate of the present embodiment, 100.0g methyl acetate, 16.5g sodium methoxide, drop in the autoclave, pass into CO gas to 4.0MPa then, reaction temperature is at At 60°C, the CO pressure was controlled at 4.0MPa. After the reaction was completed, the feed liquid was transferred to a distillation pot to distill off excess methyl acetate. Slowly add 131.4g of 10% hydrogen chloride methanol solution dropwise, control the reaction temperature at 40°C, after post-treatment, concentrate, add 0.8g p-toluenesulfonic acid to the concentrated solution, crack at 120-150°C for 6h, and finally depressurize 27.1 g of methyl 3-methoxyacrylate was obtained by rectification, with a purity of 99.2% and a yield of 77.5%. Under the action of strong base sodium alkoxide, methyl acetate makes the alpha carbon on methyl acetate form a carbanion, and then combines with carbon monoxide to form enol sodium salt aft...

Embodiment 2

[0037] Refer to attached figure 1 , a kind of preparation method of methyl 3-methoxyacrylate of the present embodiment, 200.0g methyl acetate, 16.5g sodium methoxide, drop in the autoclave, pass into CO gas to 3.5MPa then, reaction temperature is at 50°C, the CO pressure is controlled at 2.8-3.2MPa. After the reaction is over, the feed liquid is transferred to a distillation pot to distill off excess methyl acetate. Slowly add 109.3g of 10% hydrogen chloride methanol solution dropwise, the reaction temperature is 50°C, after post-treatment, concentrate, add 1.8g of sodium bisulfate to the concentrated solution, crack at 120-150°C for 6h, and finally rectify under reduced pressure Obtained, methyl 3-methoxyacrylate, 25.6 g, purity 98.9%, yield 73.0%.

Embodiment 3

[0039] Refer to attached figure 1, a kind of preparation method of methyl 3-methoxyacrylate of the present embodiment, 300.0g methyl acetate, 16.5g sodium methoxide, drop in the autoclave, pass into CO gas to 3MPa then, reaction temperature is at 50 °C, the CO pressure is controlled at 2.8-3.2MPa, after the reaction is completed, the feed liquid is transferred to a distillation pot to distill off excess methyl acetate. Slowly add 131.4g of 10% hydrogen chloride methanol solution dropwise, the reaction temperature is 45°C, after post-treatment, concentrate, add 1.3g of potassium bisulfate to the concentrated solution, crack at 120-150°C for 6h, and finally rectify under reduced pressure Obtained, methyl 3-methoxyacrylate, 29.2 g, purity 99.5%, yield 83.7%.

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Abstract

The invention discloses a preparation method of methyl 3-methoxyacrylate. The preparation method comprises the following steps: preparing a mixed solution of methyl acetate and sodium methoxide, introducing carbon monoxide into the mixed solution, carrying out heat preservation until the reaction is complete, then carrying out distillation, evaporating excessive methyl acetate, dropwise adding a hydrogen chloride methanol solution, carrying out heat preservation after the reaction is complete, and carrying out post-treatment to prepare methyl 3, 3-dimethoxy propionate, then adding a catalyst to carry out cracking reaction, and carrying out reduced pressure distillation to obtain the methyl 3-methoxyacrylate. Under the action of strong base sodium alcoholate, alpha carbon on methyl acetate forms carbon anions, then the carbon anions are combined with carbon monoxide, enol sodium salt is formed after rearrangement, the enol sodium salt and methyl alcohol are subjected to addition and substitution reactions respectively in the presence of hydrogen chloride to generate methyl 3, 3-dimethoxy propionate, and the catalyst is added for cracking reaction to obtain the methyl 3-methoxyacrylate. The reaction steps are few, the yield is high, no third-party solvent is introduced, and the redundant raw material methyl acetate can be recycled.

Description

technical field [0001] The invention belongs to the field of chemistry, in particular to a preparation method of methyl 3-methoxyacrylate. Background technique [0002] 3-Methoxymethyl acrylate (MAME) is a colorless transparent liquid, a multifunctional compound with good reactivity, and is an important C-3 building block in organic synthesis. It is widely used in pesticides, medicines and polymers In the field of materials and other fields, it is used to synthesize a variety of organic compounds. It has a wide range of uses and a large demand. However, domestic industrialization is less and most rely on imports. [0003] The synthetic method of the reported MAME has following several kinds at present: 1) Wacker catalytic oxidation method: with PdCl2 and CuCl2 as catalyst, acrylic acid and methyl alcohol are efficiently oxidized and catalyzed into 3,3-dimethoxypropionate methyl ester and 3- Methyl methoxyacrylate, the conversion rate of acrylic acid reaches 95.2%. This meth...

Claims

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Application Information

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IPC IPC(8): C07C67/31C07C67/313C07C67/327C07C67/54C07C69/734
CPCC07C67/31C07C67/313C07C67/327C07C67/54C07C69/734
Inventor 不公告发明人
Owner 昂吉(上海)环保新材料科技有限公司
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