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Method for preparing natural anisaldehyde from anethol

A kind of technology of anethole and anisaldehyde, which is applied in the field of preparation of anisaldehyde, can solve the problems of increased process complexity and unsafety, high toxicity of reaction solvent acetonitrile, complex catalyst synthesis, etc., and achieves easy recovery and reuse, high-efficiency recovery and reuse , the effect of short reaction time

Inactive Publication Date: 2014-09-10
GUANGXI UNIV FOR NATITIES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the catalyst synthesis of this process is complex and difficult to recover, and the reaction solvent acetonitrile is more toxic
In addition, using a concentration of 50% H 2 o 2 , increasing the complexity and insecurity of the process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Add 0.4g anethole and 0.005g FeVO to the 100mL round bottom flask respectively 4 , 15mL of dioxane, shake well and heat to 35°C, then add 2.5mL of 30% H 2 o 2 , Reaction 4h. After completion of the reaction, the ferric vanadate catalyst was isolated to obtain the reaction solution. The contents of anethole and anisaldehyde in the reaction solution were analyzed by gas chromatography to be 0g and 0.1948g respectively, and the conversion rate of anethole was calculated to be 100%, and the yield of the product anisaldehyde was The rate is 53%.

Embodiment 2

[0049] Add 0.4g anethole and 0.008g FeVO to the 100mL round bottom flask respectively 4 , 15mL of dioxane, shake well and heat to 35°C, then add 1.5mL of 30% H 2 o 2 , Reaction 4h. After completion of the reaction, the ferric vanadate catalyst was isolated to obtain the reaction solution. The contents of anethole and anisaldehyde in the reaction solution were analyzed by gas chromatography to be 0g and 0.2462g respectively, and the conversion rate of anethole was calculated to be 100%. The yield of product anisaldehyde was The rate is 67%.

Embodiment 3

[0051] Add 0.4g anethole and 0.004g FeVO to the 100mL round bottom flask respectively 4 , 15mL of dioxane, shake well and heat to 25°C, then add 1.5mL of 30% H 2 o 2 , Reaction 4h. After completion of the reaction, the ferric vanadate catalyst was separated to obtain the reaction solution. The content of anethole and anisaldehyde in the reaction solution by gas chromatography was analyzed to be 0.284g and 0.0849g respectively, and the conversion rate of anethole was calculated to be 29%. The yield was 23.1%.

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PUM

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Abstract

The invention discloses a method for preparing natural anisaldehyde from anethol. According to the method, anisaldehyde with a relatively high natural degree is prepared by taking anethol as a raw material and taking dioxane as a solvent through the oxidation of hydrogen peroxide under the catalysis of ferric vanadate. The method disclosed by the invention has the following characteristics: 1, the reaction condition is mild, the reaction time is short, and the process is simple; 2, inexpensive H2O2 is taken as an oxidizing agent in the reaction process; and 3, the use amount of the catalyst is small and the catalyst can be used repeatedly.

Description

technical field [0001] The invention belongs to a preparation method of chemical products. Specifically, it is a method for preparing anisaldehyde from anethole. Background technique [0002] As an important fine chemical, anisaldehyde can be widely used as a flavor because of its long-lasting hawthorn aroma. It is also an intermediate for the preparation of drugs such as amoxacarbyl penicillin, and its price is more than twice that of anethole. Industrially, anisaldehyde can be obtained by oxidation of anethole. Anisaldehyde prepared from natural anethole has the best aroma. Anethole is the main ingredient in star anise oil. my country's fennel oil is rich in resources, and its output accounts for 80% of the world's total output. Therefore, the preparation of anisaldehyde from anethole has industrial application value. [0003] The preparation of anisaldehyde from anethole mainly includes ozone oxidation, electrochemical method, manganese dioxide oxidation method and b...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C47/575C07C45/28
CPCY02P20/584
Inventor 姚兴东彭才华聂园梅石展望雷福厚
Owner GUANGXI UNIV FOR NATITIES