Synthesis method of natural anisaldehyde

A technology of natural anethole and synthesis method, which is applied in chemical instruments and methods, preparation of carbon-based compounds, preparation of organic compounds, etc., can solve the problems of high investment cost, limited promotion, etc., and achieves reduction of solid waste, cost reduction, less corrosive effect

Active Publication Date: 2020-03-17
ANHUI SHENGNUOBEI CHEM TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method has good selectivity, few by-products, high anisaldehyde yield, good quality, and easy control o

Method used

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  • Synthesis method of natural anisaldehyde
  • Synthesis method of natural anisaldehyde
  • Synthesis method of natural anisaldehyde

Examples

Experimental program
Comparison scheme
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Example Embodiment

[0022] The purpose of the present invention is to provide a method for synthesizing anisaldehyde, which includes the following steps:

[0023] Step 1: Add natural anethole, catalyst and solvent into the reaction vessel, mix and raise the temperature.

[0024] In step one, first add the anethole and solvent into the reaction vessel, stir and mix evenly, then add the catalyst, and evenly disperse in the reaction solution under stirring conditions.

[0025] In a preferred mode of the present invention, the reaction vessel is connected to a reflux device for cooling and refluxing the volatilized solvent during the heating reaction.

[0026] The purity of the natural anethole should not be less than 90%. If the content of the raw anethole is too low, the introduction of impurities from the source will cause the difficulty of extracting the product anisaldehyde, so that the purity of the product is difficult to meet the requirements for use.

[0027] The solvent is selected from ethers, such ...

Example

[0060] Example Example 1

[0061] Put 148g natural anethole (the purity of anethole is 90%) into the reaction vessel, then add 200g methanol and stir and mix well, then add 1.5g cobalt acetate, 0.5g copper acetate and 2.0g disodium hydrogen phosphate After stirring and dispersing, the reaction system was heated to 50°C, and then, after the oxygen was treated by the micro-nano bubble generator, it was introduced into the flask by the gas distributor for oxidation reaction. The oxygen flow rate was controlled at 200mL / min, and the reflux reaction was started. . Until the mass fraction of annethole <1%, stop heating, end the reaction, the reaction time is 6h. Sampling and testing the conversion rate of anisoid is 99%, and the selectivity of anisaldehyde is 90.8%.

[0062] The cobalt acetate, copper acetate and disodium hydrogen phosphate are washed out with water, and the catalyst is recovered and used for the next batch of reaction. The remaining organic solvent was subjected to a...

Example Embodiment

[0066] Example 2

[0067] The experiment was carried out according to Example 1, except that the catalyst was 1.5 g cobalt acetate, 0.5 g copper acetate and 2.0 g dipotassium hydrogen phosphate. The reaction time was 6 hours, and the product was obtained by distillation under reduced pressure to obtain 118.2 g (purity: 95.3%). The conversion rate and selectivity of anethole were 99.5% and 92.4%, respectively, and the yield of anisaldehyde was 92%.

[0068] Qualitative and quantitative analysis was performed on the components of the distillate base after the solvent separation.

[0069] The test results are shown in the following table:

[0070] Table 2 Product composition and content in Example 2

[0071]

[0072] From the experimental results in Example 1 and Example 2, it can be seen that when disodium hydrogen phosphate and dipotassium hydrogen phosphate are used as co-catalysts, the conversion rate and selectivity of the reaction system change little, indicating that the main role...

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Abstract

The invention provides a synthesis method of natural anisaldehyde. In the method, natural anethole is adopted as a raw material, oxygen or air is adopted as an oxidant, and the anisaldehyde is prepared under the action of a catalyst. The product obtained by this method has a pure aroma and excellent quality, which are obviously better than these of anisaldehyde obtained by pure chemical synthesismethods. The catalyst and solvent used in the method can be recycled and reused, thus reducing the cost and reducing generation of three wastes. The clean oxygen or air is adopted as the oxidant, thesource is wide, the reaction condition is mild, and corrosion is low, thus facilitating industrial production of the anisaldehyde.

Description

technical field [0001] The invention belongs to the technical field of spices and fine chemicals, and in particular relates to a method for synthesizing anisaldehyde. Background technique [0002] Anisaldehyde was first produced by Cahours in the 18th century when anise oil was treated with dilute nitric acid, and gradually attracted people's attention due to its unique aroma. There are many ways to synthesize anisaldehyde. It can be obtained by organic synthesis of many petrochemical raw materials, and it can also be obtained by oxidation of natural product star anise essential oil-anethole, and anisaldehyde obtained by oxidation of anethole has the best aroma. [0003] With the increasing shortage of petrochemical raw material resources and rising prices, and our country is rich in natural anethole, the production of anisaldehyde by oxidation of natural anethole can make good use of natural resources, which has gradually attracted people's attention. People use manganese ...

Claims

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Application Information

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IPC IPC(8): C07C45/36C07C47/575
CPCC07C45/36C07C47/575Y02P20/584
Inventor 陈和平保志学
Owner ANHUI SHENGNUOBEI CHEM TECH
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