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Synthesis method of natural equivalent anise alcohol

A synthetic method and equivalent technology, applied in the field of synthesis of anisyl alcohol, can solve the problems of surrounding environmental pollution, insufficient yield, low total yield, etc., and achieve the effects of cost saving, pure aroma, and innovative process route

Active Publication Date: 2014-03-19
GUANGXI WANSHAN SPICE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But still need to add reactants formaldehyde and alkali, it is easy to cause pollution to the surrounding environment, there will be residual formaldehyde in the product, and the yield is not high enough
[0007] In addition, platinum is used as a catalyst and ferrous chloride is used as a reducing agent to obtain anisyl alcohol by hydrogenation of anisaldehyde. The total yield of this process route is not high

Method used

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  • Synthesis method of natural equivalent anise alcohol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Weigh 250 grams of natural equivalent anisaldehyde, put it into the reactor, then weigh 1 gram of Raney nickel catalyst and dissolve it in 50 grams of ethanol, and put it into the reactor. Start the stirring device to stir to make the reactants mix evenly, and then inject hydrogen until the pressure is 0.15MPa, while observing the change of pressure and temperature, stop injecting hydrogen after the pressure stabilizes, and keep the temperature at about 25-30°C. After 6 hours, slowly raise the temperature to 58-60°C, keep the temperature for 32 hours, pay attention to the change of hydrogen pressure during this period, and replenish hydrogen in time to make the hydrogenation reaction stable, until no more hydrogen is absorbed, that is, the hydrogen pressure does not change. until. After the hydrogenation reaction is completed, the semi-finished liquid anisyl alcohol is discharged. Slowly open the discharge valve of the reaction kettle, the feed liquid is discharged und...

Embodiment 2

[0025] Weigh 250 grams of natural equivalent anisaldehyde, put it into the reactor, then weigh 0.95 grams of Raney nickel catalyst, dissolve it in 50 grams of ethanol, and put it into the reactor. Start the stirring device to stir, so that the reactants are evenly mixed, inject hydrogen until the pressure is 0.12MPa, observe the changes in pressure and temperature, stop injecting hydrogen after the pressure stabilizes, and keep the temperature at about 25-30°C, After 6 hours, slowly raise the temperature to 55-60°C, and keep it warm for 33 hours. During this period, pay attention to the change of hydrogen pressure, and replenish hydrogen in time to make the hydrogenation reaction stable, until no more hydrogen is absorbed, that is, the hydrogen pressure does not change. until. After the hydrogenation reaction is completed, the semi-finished liquid anisyl alcohol is discharged. Slowly open the discharge valve of the reaction kettle, the feed liquid is discharged under the acti...

Embodiment 3

[0028] Weigh 250 grams of natural equivalent anisaldehyde, put it into the reactor, then weigh 1.03 grams of Raney nickel catalyst, dissolve it in 49 grams of ethanol, and put it into the reactor. Start the stirring device to stir, so that the reactants are mixed evenly, and the hydrogen gas is introduced until the pressure is 0.12-0.15 MPa. While observing the changes in pressure and temperature, stop the hydrogen gas injection after the pressure stabilizes, and keep the temperature at 26-30 °C After about 6 hours, slowly increase the temperature to 55-58°C, and keep the temperature for 31 hours. During this period, pay attention to the change of hydrogen pressure, and replenish hydrogen in time to make the hydrogenation reaction proceed stably until no more hydrogen is absorbed, that is, the hydrogen pressure does not increase. until it changes. After the hydrogenation reaction is completed, the semi-finished liquid anisyl alcohol is discharged. Slowly open the discharge va...

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Abstract

The invention discloses a synthesis method of natural equivalent anise alcohol. The synthesis method comprises the steps of carrying out a catalytic hydrogenation reaction on natural equivalent anisic aldehyde used as a raw material in ethanol with Raney nickel as a catalyst to obtain an anise alcohol semi-finished product, and distilling under reduced pressure to obtain a high-purity anise alcohol product. The synthesis method disclosed by the invention has the characteristics that the total reaction yield is not less than 96.0%, the purity of natural equivalent anise alcohol is up to more than 98.0%, and the catalyst can be recycled more than 35 times; and the synthesis method has the advantages of short process route, low energy consumption, environmental friendliness and the like.

Description

technical field [0001] The invention belongs to the technical field of spices and fine chemicals, and in particular relates to a synthesis method of anisyl alcohol. Background technique [0002] Natural equivalents refer to substances produced by synthetic methods, or substances processed from natural raw materials by chemical methods, whose chemical structure and properties are equivalent to those existing in natural products. [0003] The natural equivalent anisaldehyde refers to the extraction of star anise oil from the fruit and branches of the natural plant star anise tree, and the star anise oil is purified to obtain anethole, which is oxidized to synthesize anisaldehyde, which can be used as a raw material for the synthesis of anisyl alcohol. [0004] Anisyl alcohol, also known as p-methoxybenzyl alcohol, anisyl alcohol, 4-methoxybenzyl alcohol, p-methoxybenzyl alcohol, 4-methoxybenzyl alcohol, p-methoxybenzyl alcohol, is colorless at room temperature Or light yellow...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C43/23C07C41/26
CPCY02P20/584
Inventor 杨少凡刘新伟文天寿胡林刚赖积南黄江涛
Owner GUANGXI WANSHAN SPICE
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