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Preparation process of ethyl p-methoxycinnamate

A technology of ethyl cinnamate and preparation process, which is applied in the preparation of carboxylate, the preparation of organic compounds, the separation/purification of carboxylate, etc., can solve the problems of high heating temperature, complicated operation, low esterification rate and the like, Achieve the effect of increasing solubility, high yield and improving synthesis yield

Pending Publication Date: 2022-05-06
ZITONG HUIQUAN PERFUME CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the synthetic method of synthesizing ethyl p-oxymethyl cinnamate mainly contains following several kinds, one is to utilize Perkin condensation reaction or Knoevenagle reaction to synthesize and obtain cinnamic acid, obtain cinnamate ester through esterification again, above two kinds of reactions all need Cinnamate is prepared by two-step reaction, and the esterification rate is low; the second is that the patent CN 107602384A prepares p-oxymethylbenzaldehyde and diethyl malonate under the action of a solid superbase to obtain a light yellow solid, which is Ethyl p-oxymethylbenzoate
However, the heating temperature of the solid superbase used in the reaction is as high as 500-600°C, and active metal sodium is required. The preparation process is complicated and has low safety.

Method used

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  • Preparation process of ethyl p-methoxycinnamate
  • Preparation process of ethyl p-methoxycinnamate
  • Preparation process of ethyl p-methoxycinnamate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1～4

[0041] Embodiment 1~4 is the solvent screening experiment in the step 1, and its concrete operation is: 1, feed intake, 500Kg ethyl acetate, 140Kg sodium ethylate and solvent 280Kg are added to reactor, stir;

[0042] 2. Reaction: Add 200Kg of anisaldehyde dropwise while stirring, and control the reaction temperature at about 45°C. After the dropwise addition, keep the temperature at 40-45°C for one hour, and take a sample test. The reference content of the product is about 95%, that is, the reaction is complete ;

[0043] 3. Washing and flashing treatment: add water to the reaction kettle, and then add 13% sulfuric acid to neutralize the alkali. Then add water to remove the salt in the organic phase, separate the liquids, transfer the organic phase to the still, the temperature of the still does not exceed 90°C, remove the solvent, and send it to the flash tank for flashing to obtain the flash feed liquid. The temperature is 110~125℃;

[0044] 4. Crystallization, centrifuga...

Embodiment 5～8

[0048]Examples 5-8 are: when the solvent in step 1 is cyclohexane, the influence of the feeding ratio of cyclohexane to anisaldehyde on the reaction yield.

[0049] Its specific operation is: 1, feeding materials, 500Kg ethyl acetate, 140Kg sodium ethylate and a certain amount of cyclohexane are added to the reactor, and stirred;

[0050] 2. Reaction: Add 200Kg of anisaldehyde dropwise while stirring, and control the reaction temperature at about 45°C. After the dropwise addition, keep the temperature at 40-45°C for one hour, and take samples for testing. The reference content of the product is about 95%, that is, the reaction complete;

[0051] 3. Washing and flashing treatment: add water to the reaction kettle, and then add 13% sulfuric acid to neutralize the alkali. Then add water to remove the salt in the organic phase, separate the liquids, transfer the organic phase to the still, the temperature of the still does not exceed 90°C, remove the solvent, and send it to the f...

Embodiment 9～12

[0057] Embodiment 9~12 is the alkali screening experiment in the step 1, and its concrete operation is: 1, feeds intake, 500Kg ethyl acetate, 140Kg alkali and cyclohexane 280Kg are added reactor, stir;

[0058] 2. Reaction: Add 200Kg of anisaldehyde dropwise while stirring, and control the reaction temperature at about 45°C. After the dropwise addition, keep the temperature at 40-45°C for one hour, and take a sample test. The reference content of the product is about 95%, that is, the reaction is complete ;

[0059] 3. Washing and flashing treatment: add water to the reaction kettle, and then add 13% sulfuric acid to neutralize the alkali. Then add water to remove the salt in the organic phase, separate the liquids, transfer the organic phase to the still, the temperature of the still does not exceed 90°C, remove the solvent, and send it to the flash tank for flashing to obtain the flash feed liquid. The temperature is 110~125℃;

[0060] 4. Crystallization, centrifugation an...

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Abstract

Ethyl p-methoxycinnamate has wide application in the fields of preparation of sunscreen products, antifungal agents and food additives. The invention provides a preparation process for synthesizing p-oxygen methyl ethyl cinnamate by using a natural product anisic aldehyde as a reactant to react with ethyl acetate in one step, the preparation process is simple in reaction, high in safety and easy to operate, a large amount of p-oxygen methyl ethyl cinnamate can be prepared, and the finally obtained p-oxygen methyl ethyl cinnamate is a white solid and has a wide application prospect. The purity can reach 99.98%.

Description

technical field [0001] The invention relates to the field of compound preparation, in particular to a preparation process of ethyl p-methoxycinnamate. Background technique [0002] Cinnamic acid lipids are widely used in the fields of fine chemicals and pharmaceuticals. Ethyl p-oxymethyl cinnamate, derived from Kaempfera extract, has become an ideal sunscreen because of its good absorption in the 280-320nm region, high absorption rate, no irritation to the skin, and good safety. agent, and has a certain biological activity, with antifungal effect. At the same time, in life, ethyl p-methoxycinnamate is also used as a food flavor additive because of its unique fragrance, so ethyl p-methoxycinnamate has an important role in the preparation of sunscreen products, antifungal agents, and food additives. Wide range of applications. [0003] At present, the synthetic method of synthesizing ethyl p-oxymethyl cinnamate mainly contains following several kinds, one is to utilize Perk...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/343C07C69/734C07C67/48C07C67/54
CPCC07C67/343C07C67/48C07C67/54C07C69/734
Inventor 钟利明郭祥东
Owner ZITONG HUIQUAN PERFUME CHEM