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Method for preparation of menthone

A technology of menthone and isopulegol, which is applied in the field of preparation of menthone, can solve the problems of low reaction cost, etc., and achieve the effects of reducing the introduction of impurities, high catalytic activity, and easy recovery

Active Publication Date: 2018-02-23
WANHUA CHEM GRP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The object of the present invention is to provide a kind of method for preparing menthone, thus solve many problems existing in the existing preparation process of menthone, the present invention utilizes palladium-ruthenium catalyst to heterogeneously catalyze isopulegol under mild reaction conditions Menthone can be prepared in high yield, the catalyst can be recovered in a convenient way, it has a simpler reaction process, lower reaction cost, good environmental friendliness, and has better industrialization prospects

Method used

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Effect test

Embodiment 1

[0045] Pd(PPh 3 ) 4 (260mg, 0.225mmol), dichloro(p-methylcymenyl)ruthenium(II) dimer (275.57mg, 0.450mmol), tetraethylglycol (418mg, 2.20mmol), sec-butanol Add aluminum (9.50g, 38.5mmol) and 1-butanol (3ml, 32.7mmol) into a 50ml round bottom flask with a condenser, and stir at 120°C for 10h to form a suspension. 2ml of pure water was added dropwise, and the reaction mixture was stirred at 120°C for 30 min. The solid catalyst was screened out, washed with acetone, and then dried in air at room temperature to obtain a powder catalyst.

Embodiment 2

[0047]Bis(dibenzylideneacetone)palladium (258.75mg, 0.450mmol), dichloro(p-methylisopropylphenyl)ruthenium(II) dimer (275.57mg, 0.450mmol), tetraethylethylenedi Add alcohol (418mg, 2.20mmol), aluminum sec-butoxide (9.50g, 38.5mmol), 1-butanol (3ml, 32.7mmol) into a 50ml round bottom flask with a condenser, stir at 120°C for 10h, and prepare into a suspension. 2ml of pure water was added dropwise, and the reaction mixture was stirred at 120°C for 30 min. The solid catalyst was screened out, washed with acetone, and then dried in air at room temperature to obtain a powder catalyst.

Embodiment 3

[0049] Pd[(t-Bu) 3 P] 2 (260mg, 0.225mmol), [Ru(COD)](ClO 4 ) 2 (275.51mg, 0.675mmol), tetraethylethylene glycol (418mg, 2.20mmol), aluminum sec-butoxide (9.50g, 38.5mmol), 1-butanol (3ml, 32.7mmol) were added to a 50ml In a round bottom flask, stir at 120°C for 10h to make a suspension. 2ml of pure water was added dropwise, and the reaction mixture was stirred at 120°C for 30 min. The solid catalyst was screened out, washed with acetone, and then dried in air at room temperature to obtain a powder catalyst.

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Abstract

The invention discloses a method for the preparation of menthone. A palladium-ruthenium catalyst is used for heterogeneous catalysis under mild conditions, and isopulegol is used for the preparation of the menthone. The palladium-ruthenium catalyst can be used for efficiently catalyzing the isopulegol and making the isopulegol convert into menthone under the mild conditions.

Description

technical field [0001] The invention belongs to the field of preparation of menthone, in particular to a method for preparing menthone by heterogeneous catalysis of isopulegol. 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, is mainly used to prepare mint-type flavors, so the synthesis of menthone has always been subject to people's attention. [0003] Patent US3124614 reports that menthone can be obtained by hydrogenating thymol under the action of Pd catalyst, but the raw material thymol is not easy to obtain, the reaction conditions are harsh, and the requirements for equipment are high. [0004] Patent CN106061933A reports a method for preparing menthone by contacting isopulegol in the gas phase with an activated oxidative copper catalyst. In this method, the copper cataly...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/00C07C49/407B01J31/22B01J31/24
CPCB01J31/2291B01J31/2404B01J2231/763B01J2531/821B01J2531/824C07C29/172C07C45/002C07C49/407C07C35/08
Inventor 王亚新董菁黄文学张永振黎源鲍元野王联防于磊李晶杨洗李文滨
Owner WANHUA CHEM GRP CO LTD
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