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Preparation method of methyl 3, 3-dimethoxy propionate

A technology of methyl dimethoxypropionate and methyl acetate, applied in the chemical field, can solve the problems of low yield, high cost, complicated preparation process, etc., and achieve the effect of high yield, few reaction steps and simple operation

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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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to solve the existing 3,3-dimethoxy methyl propionate preparation process complex, high cost and low yield problems

Method used

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  • Preparation method of methyl 3, 3-dimethoxy propionate

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Embodiment 1

[0032] Refer to attached figure 1 , a preparation method of methyl 3,3-dimethoxypropionate in this embodiment, put 100.0g methyl acetate and 16.5g sodium methoxide into the autoclave, and then feed CO gas to 4.0MPa , the reaction temperature is at 60°C, and the CO pressure is controlled at 4.0MPa. After the reaction is over, the feed liquid is transferred to a distillation pot to evaporate excess methyl acetate. Slowly add 131.4g of 10% methanolic hydrogen chloride solution dropwise, and control the reaction temperature to 40°C. After post-treatment, concentration and distillation, 39.0g of methyl 3,3-dimethoxypropionate is obtained, with a purity of 96.8%. The rate is 85.2%. 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 after rearrangement. The enol sodium salt undergoes addition and substitution reactions with methanol in the presence...

Embodiment 2

[0034] Refer to attached figure 1 , a preparation method of methyl 3,3-dimethoxypropionate in this embodiment, put 200.0g methyl acetate and 16.5g sodium methoxide into the autoclave, and then feed CO gas to 3.5MPa , the reaction temperature is 50°C, and 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 evaporate excess methyl acetate. Slowly add 109.3g of 10% hydrogen chloride methanol solution dropwise, the reaction temperature is 50°C, after post-treatment, concentration, distillation, to obtain 3,3-dimethoxypropionate methyl ester, 36.5g, purity 97.5%, yield 80.2%.

Embodiment 3

[0036] Refer to attached figure 1 , a preparation method of methyl 3,3-dimethoxypropionate in this embodiment, 300.0g methyl acetate and 16.5g sodium methoxide are put into the autoclave, and then CO gas is introduced to 3MPa, The reaction temperature is 50°C, and 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 evaporate excess methyl acetate. Slowly add 131.4g of 10% hydrogen chloride methanol solution dropwise, the reaction temperature is 45°C, after post-treatment, concentration, distillation, to obtain 3,3-dimethoxypropionate methyl ester, 41.6g, purity 97.1%, yield 91.0%.

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Abstract

The invention discloses a preparation method of 3, 3-dialkoxy propionate. The preparation method of 3, 3-dialkoxy propionate comprises the following steps: introducing carbon monoxide into a metal alkoxide solution of ester, and keeping the temperature until the reaction is complete; and evaporating to remove excessive ester, dropwise adding an alcoholic solution of hydrogen chloride, preserving heat and reacting completely, and then carrying out post-treatment to prepare 3, 3-dialkoxy propionate. The preparation method has the advantages that the reaction steps are few, the operation is simple, the yield is high, a third-party solvent is not introduced, redundant raw material ester can be recycled, and the cost is further saved.

Description

technical field [0001] The invention belongs to the field of chemistry, and specifically relates to a preparation method of methyl 3,3-dimethoxypropionate. Background technique [0002] Methyl 3,3-dimethoxypropionate can be used as chemical reagents, fine chemicals, pharmaceutical intermediates, material intermediates, etc. A kind of main application of 3,3-dimethoxypropionate methyl ester is to synthesize coumarin and its derivatives etc., for example can prepare coumarin, scopoletin (7-hydroxyl-6-methoxycoumarin ), isoscypoletin (6-hydroxy-7-methoxycoumarin). Coumarin and its derivatives are used in the deployment of industrial and daily tobacco flavors, are excellent fixatives, and are also used in electroplating and other industries. Coumarin drugs have anticoagulant, antitumor, antithrombotic, antiosteoporosis effects, protect the liver, and regulate anti-sleep. Therefore, methyl 3,3-dimethoxypropionate has wide application and market value. [0003] However, the ex...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/708C07C67/31C07C67/48C07C67/54
CPCC07C67/31C07C67/48C07C67/54C07C67/313C07C69/708C07C69/732C07C69/738
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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