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Synthesis method of anethole

A synthesis method and technology of synthesis reaction, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of difficult promotion, harsh equipment requirements, high cost, low temperature, reduced requirements, and mild reaction conditions. Effect

Active Publication Date: 2013-03-27
成都建中香料香精有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the method of using a strong acid as a medium to react and catalyze the dehydration of p-methoxyphenylpropanol to obtain anethole at high temperature is more demanding on equipment, and industrial production is not only costly, but also difficult to promote in industry; In the way of using expensive dehydration catalysts (such as titanium dioxide), although the catalyst can be regenerated and recycled after subsequent treatment, because the catalyst itself is expensive, the production cost is still high if the industrial production method is adopted

Method used

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  • Synthesis method of anethole
  • Synthesis method of anethole
  • Synthesis method of anethole

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Take each material according to the following weight ratio:

[0039] p-methoxyphenylpropanol 500kg

[0040] Dehydrating agent - anhydrous sodium sulfate 1kg

[0041] With water agent - toluene 1500kg

[0042] Put the weighed dehydrating agent and water-carrying agent in the reaction kettle, stir and mix and heat to 100°C to reflux, then add p-methoxyphenylpropanol dropwise to the reflux mixture, and control the dropping time to 6-8 Hours; after the dropwise addition of p-methoxyphenylpropanol, keep the temperature between 100-150°C for 30min-2 hours, and stop the reaction when no water flows out of the water separator.

[0043] The above reaction mixture was sampled and detected by LC / MS, and the reaction conversion rate was 90.2%; the obtained reaction mixture was post-processed to obtain 400 kg of the product anethole, and the product yield was 90.1%.

Embodiment 2

[0045] Take each material according to the following weight ratio:

[0046] p-methoxyphenylpropanol 500kg

[0047] Dehydrating agent - anhydrous magnesium sulfate 1kg

[0048] With water agent - benzene 4000kg

[0049]Put the weighed dehydrating agent and water-carrying agent in the reaction kettle, stir and mix and heat to 80°C to reflux, then add p-methoxyphenylpropanol dropwise to the reflux mixture, and control the dropping time to be 6-8 Hours; after the dropwise addition of p-methoxyphenylpropanol, keep the temperature between 90-150°C for 30min-2 hours, and stop the reaction when no water flows out of the water separator.

[0050] The above reaction mixture was sampled and detected by LC / MS, and the reaction conversion rate was 90.6%; the obtained reaction mixture was post-processed to obtain 401 kg of anethole product, and the product yield was 90.1%.

Embodiment 3

[0052] Take each material according to the following weight ratio:

[0053] p-methoxyphenylpropanol 800kg

[0054] Dehydrating agent - calcium hydride 1kg

[0055] With water agent - p-xylene 2400kg

[0056] Put the weighed dehydrating agent and water-carrying agent in the reaction kettle, stir and mix and heat to 115°C to reflux, then add p-methoxyphenylpropanol dropwise to the reflux mixture, and control the dropping time to be 6-8 Hours; after the dropwise addition of p-methoxyphenylpropanol, keep the temperature between 120-150°C for 30min-2 hours, and stop the reaction when no water flows out of the water separator.

[0057] The above reaction mixture was sampled and detected by LC / MS, and the reaction conversion rate was 90.3%; the obtained reaction mixture was post-processed to obtain 634 kg of anethole, and the product yield was 89.1%.

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Abstract

The invention discloses a preparation method of chemical spices, and specially relates to a synthesis method of anethole. The synthesis method comprises the step of jointly reacting p-anisole propanol with a dehydrating agent and a water-carrying agent at a temperature of 90-150 DEG C, so that anethole, namely, p-allylanisole esdragol is synthesized. The synthesis method of anethole disclosed by the invention can simultaneously guarantee the reaction conversion rate and significantly reduce the requirements on reaction equipment, thereby effectively reducing the production costs thereof in industrial applications.

Description

technical field [0001] The invention relates to a method for preparing chemical spices, in particular to a method for synthesizing anethole. Background technique [0002] Anethole, whose chemical name is p-propenyl anisole, is a commonly used chemical plant spice, and its structure is shown in the figure below: [0003] [0004] The preparation of existing anethole generally adopts the method of separating or chemically synthesizing from natural plants, and the production of products obtained by the preparation method of separating and obtaining anethole from natural plants is small, and the cost of raw materials is relatively high; the existing chemical synthesis prepares anethole The method is mainly to obtain the product anethole, i.e. p-propenyl anisole, after carrying out dehydration reaction to p-methoxyphenylpropanol; the reaction process of the above-mentioned chemical synthesis is as follows: [0005] [0006] In order to allow the raw material p-methoxypheny...

Claims

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Application Information

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IPC IPC(8): C07C43/215C07C41/18
Inventor 李永红李良龙许琨曾林久马妙玲黄宗凉方大庆廖英陈军周锦
Owner 成都建中香料香精有限公司
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