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Catalytic synthesis method of methyl cinnamate

A technology of methyl cinnamate and a synthesis method, applied in the field of supported catalysts, can solve the problems of waste liquid polluting the environment, many side reactions, troublesome post-processing, etc., and achieve the effects of simplifying operation steps, reducing production costs, and being easier to separate

Inactive Publication Date: 2012-10-03
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The traditional method for synthesizing methyl cinnamate is inorganic acid (such as hydrochloric acid, sulfuric acid) catalyzed esterification method, but this method has many side reactions (such as sulfonation, oxidation, addition, carbonization, etc.), and the product yield and quality are low. Severe corrosion of equipment, troublesome post-processing and environmental pollution by waste liquid, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Take 14.8g of cinnamic acid, 12.8g of methanol and 0.74g of supported acidic catalyst into a 250ml flask, heat to reflux for 3h, and then carry out vacuum distillation until no liquid is distilled out. Filtrate while hot to remove the solid catalyst and maintain the liquid phase temperature at 43°C. Add 6% K dropwise to the product 2 CO 3 Solution, until the pH of the solution is 8.5, while maintaining the solution temperature at 43 ° C, standing for stratification, removing the water phase, washing the product with twice the volume of 42 ° C deionized water, standing for stratification, removing the water phase, and repeating this step until the pH of the solution was 7. Three volumes of deionized water at 10° C. was added to the product under constant stirring, and a pale yellow solid was precipitated, namely methyl cinnamate, with a yield of 86%.

Embodiment 2

[0016] Take 14.8g of cinnamic acid, 25.6g of methanol and 0.85g of supported acid catalyst into a 250ml flask, heat to reflux for 4h, and then carry out vacuum distillation until no liquid is distilled out. Filtrate while hot to remove the solid catalyst and maintain the liquid phase temperature at 40°C. Add 9% K dropwise to the product 2 CO 3 Solution, until the pH of the solution is 8, while maintaining the solution temperature at 40 ° C, standing for stratification, removing the water phase, washing the product with twice the volume of 41 ° C deionized water, standing for stratification, removing the water phase, and repeating this step To the pH value of the solution is 7.2. Three volumes of deionized water at 9° C. was added to the product under constant stirring, and a pale yellow solid was precipitated, namely methyl cinnamate, with a yield of 91%.

Embodiment 3

[0018] Take 14.8g of cinnamic acid, 14.6g of methanol and 4.44g of supported acid catalyst into a 250ml flask, heat to reflux for 6h, and then carry out vacuum distillation until no liquid is distilled out. Filtrate while hot to remove the solid catalyst and maintain the liquid phase temperature at 50°C. Add 5% K dropwise to the product 2 CO 3 Solution, until the pH of the solution is 8.2, while maintaining the solution temperature at 50 ° C, standing for stratification, removing the water phase, washing the product with twice the volume of 40 ° C deionized water, standing for stratification, removing the water phase, and repeating this step until the pH of the solution was 7. Three volumes of deionized water at 5° C. was added to the product under constant stirring, and a pale yellow solid was precipitated, namely methyl cinnamate, with a yield of 88%.

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Abstract

The invention relates to a method for preparing methyl cinnamate. Cinnamic acid and methanol are subjected to liquid-solid-phase catalytic esterification reaction under the action of a supported catalyst to prepare the methyl cinnamate. By controlling the reaction technique conditions and purification technique conditions, the product is purified with deionized water at different temperatures, thereby obtaining the high-yield high-purity methyl cinnamate at low cost.

Description

technical field [0001] The invention relates to a catalytic synthesis method of methyl cinnamate, in particular to a method for synthesizing a target product through a liquid-solid phase catalytic reaction using a supported catalyst. Background technique [0002] Methyl cinnamate, also known as β-phenyl acrylate methyl ester, has a cocoa aroma and is a white to light yellow crystal or colorless to light yellow liquid with a melting point of 34-38°C. It is insoluble in water but soluble in ether. It is an important It is mainly used in the daily chemical and food industries. It is a commonly used fixative and food flavor, and it is also an important organic synthesis raw material. [0003] The traditional method for synthesizing methyl cinnamate is inorganic acid (such as hydrochloric acid, sulfuric acid) catalyzed esterification method, but this method has many side reactions (such as sulfonation, oxidation, addition, carbonization, etc.), and the product yield and quality a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/618C07C67/08
Inventor 曾作祥崔丽薛为岚高石秀袁明轩
Owner EAST CHINA UNIV OF SCI & TECH
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