A method for preparing high-purity l-menthone

A menthone, high-purity technology, applied in the field of preparation of high-purity L-menthone, can solve the problems of low reaction cost, etc., and achieve the effects of good activation of free radicals, good catalytic performance, remarkable operability and economy

Active Publication Date: 2021-10-22
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of the present invention is to provide a method for preparing high-purity L-menthone, thereby solving many problems existing in the existing preparation process of menthone. The present invention utilizes a ruthenium catalyst loaded on a solid base under mild reaction conditions Heterogeneous catalysis of L-isopulegol to prepare L-menthone with high yield, the catalyst can be recovered in a convenient way, with a simpler reaction process, lower reaction cost, good environmental friendliness, and a process through hydrogenation transfer No need to use hydrogen, better process safety, and better industrialization prospects

Method used

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  • A method for preparing high-purity l-menthone
  • A method for preparing high-purity l-menthone
  • A method for preparing high-purity l-menthone

Examples

Experimental program
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Effect test

Embodiment 1

[0056] 1) Ultrasonic disperse 0.852g graphene oxide in 106.5mL ethanol, under the protection of nitrogen, slowly add 42.6mg (0.289mmol) tetraethylammonium hydroxide while stirring, heat the oil bath to 100°C and reflux for 24h, cool, Suction filtration, washing with ethanol for 6 times, and drying in a vacuum oven overnight to obtain graphene solid powder loaded with tetraethylammonium hydroxide.

[0057] 2) Disperse 0.895g of graphene solid powder loaded with tetraethylammonium hydroxide prepared in step 1) in 111.875mL of absolute ethanol, slowly add 12mg (0.058mmol) of RuCl 3 , and the mixture was stirred at room temperature for 24h. After the reaction is completed, filter with suction, wash with a large amount of absolute ethanol and deionized water, and dry the obtained filter cake at 70° C. for 24 hours. After drying, it is ground to a powder for future use, which is recorded as a ruthenium catalyst supported on a solid organic base. A total of 0.907 g of catalyst was ...

Embodiment 2

[0059] 1) Ultrasonic disperse 0.912g graphene oxide in 91.28mL ethanol, under the protection of nitrogen, slowly add 73mg (1.301mmol) potassium hydroxide while stirring, heat the oil bath to 110°C and reflux for 24h, cool, filter with Washed with ethanol for 6 times, and dried overnight in a vacuum oven to obtain a graphene solid powder loaded with potassium hydroxide.

[0060] 2) Disperse 0.986g of graphene solid powder loaded with potassium hydroxide prepared in step 1) in 98.6mL of absolute ethanol, slowly add 18mg (0.087mmol) of RuCl 3 , and the mixture was stirred at room temperature for 24h. After the reaction is completed, filter with suction, wash with a large amount of absolute ethanol and deionized water, and dry the obtained filter cake at 70° C. for 24 hours. After drying, it is ground to a powder for future use, which is recorded as a ruthenium catalyst supported on a solid inorganic base. A total of 1 g of catalyst was obtained, the mass fraction of ruthenium w...

Embodiment 3

[0062] 1) Ultrasonic disperse 0.8g graphene oxide in 88.84mL ethanol, under the protection of nitrogen, slowly add 80mg (0.579mmol) potassium carbonate while stirring, heat the oil bath to 120°C and reflux for 24h, cool, filter with ethanol, After washing 6 times, the vacuum oven was dried overnight to obtain a graphene solid powder loaded with potassium carbonate.

[0063] 2) Disperse the 0.88g graphene solid powder loaded with potassium carbonate prepared in step 1) in 97.7mL absolute ethanol, slowly add 6mg (0.029mmol) of RuCl 3 , and the mixture was stirred at room temperature for 24h. After the reaction is completed, filter with suction, wash with a large amount of absolute ethanol and deionized water, and dry the obtained filter cake at 70° C. for 24 hours. After drying, it is ground to a powder for future use, which is recorded as a ruthenium catalyst supported on a solid inorganic base. A total of 0.886 g of catalyst was obtained, the mass fraction of ruthenium eleme...

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Abstract

The invention discloses a method for preparing high-purity L-menthone. In the method, under the action of a solid base-supported ruthenium catalyst, raw material L-isopulegol is subjected to a heterogeneous catalytic reaction to obtain high-purity L-menthone as a product. The present invention utilizes the ruthenium catalyst supported on the solid base to catalyze L-isopulegol with a high yield to prepare L-menthone under mild reaction conditions, the catalyst can be recovered in a convenient manner, and the reaction process is simpler. Low reaction cost, good environmental friendliness, no need to use hydrogen in the hydrogenation transfer process, and better process safety and industrialization prospects.

Description

technical field [0001] The invention belongs to the field of menthone preparation, in particular to a method for preparing high-purity L-menthone. Background technique [0002] Menthone, also known as menthone, has the cool and characteristic aroma of natural mint. Menthone exists in the form of two stereoisomers: menthone and isomenthone, each of which exists in the form of two enantiomers, and is mainly used to prepare mint-type flavors. The currently disclosed preparation methods are as follows: A few kinds: [0003] Patent US3124614 uses thymol to hydrogenate under the action of Pd catalyst to obtain menthone, but the raw material thymol is not easy to obtain, the reaction conditions are harsh, the requirements for equipment materials are high, and the equipment cost is expensive. [0004] Patent CN106061933A discloses a method for preparing menthone by contacting isopulegol in the gas phase with an activated oxidizing copper catalyst. In this method, the copper cataly...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C49/407C07C45/29B01J23/46
CPCB01J23/462C07B2200/07C07B2200/09C07C45/29C07C49/407Y02P20/584
Inventor 王亚新方文娟于磊董菁李文滨迟森森王文李晶
Owner WANHUA CHEM GRP CO LTD
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