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Method for preparing anise acid with anise camphor

A technology of anisole and anisic acid, which is applied in the field of preparing anisic acid by using anisole, can solve the problems of excessive heavy metal content in organic solvent residues, application restrictions, etc. Effect

Inactive Publication Date: 2014-02-12
广西辰康生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Anisic acid is traditionally produced by petroleum synthesis routes. During the production process, organic solvents such as ethyl acetate and ethanol are commonly used for crystallization and recrystallization. Due to the risk of excessive heavy metal content and residual organic solvents, it is widely used in food, medicine, cosmetics, etc. The application in the field is limited, and it is an inevitable trend and requirement to seek the production technology of natural grade anisic acid from natural raw materials

Method used

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  • Method for preparing anise acid with anise camphor
  • Method for preparing anise acid with anise camphor
  • Method for preparing anise acid with anise camphor

Examples

Experimental program
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Effect test

Embodiment 1

[0064] Add 10g of anethole, 240ml of water, and 10g of NaOH into a 1000ml flask equipped with a reflux condenser, a thermometer, and a dropping funnel, heat it to 80°C in a stirring water bath, and then add dropwise a total of 295ml of anethole with a mass percentage concentration of 30% to the flask. h 2 o 2 , Control the rate of addition, 4h dropwise, and then stir the reaction for 5h, the reaction is terminated. After the reaction, cool to room temperature, add concentrated hydrochloric acid until the pH is 2, filter, wash the filter cake with water until neutral, and dry to constant weight at 105°C to obtain 8.13 g of anilic acid product, with a yield of 81.3%.

Embodiment 2

[0066] Add 10g of anethole, 180ml of water, and 6g of NaOH into a 1000ml flask equipped with a reflux condenser, a thermometer, and a dropping funnel, heat it to 80°C in a stirring water bath, and then add dropwise a total of 230ml of anethole with a mass percentage concentration of 30% to the flask. h 2 o 2 , Control the rate of addition, 4h dropwise, and then stir the reaction for 4h, the reaction is terminated. After the reaction, cool to normal temperature, add concentrated hydrochloric acid until the pH is 2, filter, wash the filter cake with water until neutral, and dry to constant weight at 105°C to obtain 6.20 g of anilic acid product, with a yield of 62.0%.

Embodiment 3

[0068] Add 10g of anethole, 60ml of water, and 4g of NaOH into a 500ml flask equipped with a reflux condenser, a thermometer, and a dropping funnel, heat it to 80°C in a stirring water bath, and then add dropwise a total of 150ml of anethole with a mass percentage concentration of 30% to the flask. h 2 o 2 , Control the rate of addition, 4h dropwise, and then stir the reaction for 3h, the reaction is terminated. After the reaction, cool to normal temperature, add concentrated hydrochloric acid until the pH is 2, filter, wash the filter cake with water until neutral, and dry to constant weight at 105°C to obtain 5.0 g of anilic acid product, with a yield of 50.0%.

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Abstract

The invention discloses a method for preparing anise acid with anise camphor. Anise acid is prepared by performing oxidation treatment on the anise camphor with an H2O2 solution in an alkaline solution. In the method, no organic solvent is used in reaction and separation processes; anise acid has no toxic or harmful solvent residue; the method can be used for the industries of medicine, food and cosmetics, and is mild in reaction condition, simple in purification and refining, easy and simple to operate, and high in product purity; H2O2 serves as an oxidant; a reaction product is water; the oxidant is green and environment-friendly; H2O2 is injected by dropwise adding to participate in reaction, so that a risk caused by sharp free radical reaction of H2O2 can be avoided effectively; a used raw material is wide in source; a catalyst is small in consumption, cheap, and easy to obtain.

Description

technical field [0001] The invention relates to the production field of anisic acid, in particular to a method for preparing anisic acid by using anethole. Background technique [0002] Anisic acid, also known as 4-methoxybenzoic acid, 4-anisic acid, 4-carboxyanisole, the English name is p-Anisic acid or 4-methoxybenzoic acid, CAS NO.: 100-09-4, FEMA NO.: 3945, the structural formula is: [0003] [0004] Natural anisic acid exists in guava, guava, anise, soda cheese, cocoa, cumin, custard apple, vanilla and star anise, but due to the low content, it is difficult to separate and purify, and the production cost is high , has no production value. Anisic acid has a wide range of uses, especially in the fields of food, medicine, and cosmetics, and has developed rapidly in recent years. [0005] For example, in the fragrance and flavor industry, it is used in cocoa and creamy vanilla flavors, as well as in licorice, berry and tropical fruit flavors. Dosage (usual / maximum, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C65/21C07C51/285
CPCC07C51/285
Inventor 何春茂陈海春曹祖仁李华杰朱金忠邓倩玉增广
Owner 广西辰康生物科技有限公司
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