Method for preparing N-ethyl-2-isopropyl-5-methycyclohexane

A technology of methylcyclohexanecarboxamide and isopropyl, which is applied in the field of amide preparation, can solve the problems of increasing the difficulty of production operations, strict reaction conditions, and low yield, and achieve reduced production costs, simple operations, and environmental pollution Reduced effect

Active Publication Date: 2009-12-02
ANHUI FENGLE PERFUME
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, the patent of "High Efficiency Refrigerant--Preparation Method of Amidated Natural Menthol" with publication number CN1613845 discloses the preparation of amide from menthol through processes such as chlorination, Grignard reaction, acidification, acyl chloride, amidation, and recrystallization. Natural menthol; The disadvantage of this method is that the reaction conditions are strict in the acidification step, and the yield is low
For example, in the article "Synthesis of cooling agent N

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] (1) Preparation of Menthyl Magnesium Chloride

[0016] According to the molar ratio of menthyl chloride:magnesium 1:2, put the menthyl chloride into tetrahydrofuran of 3 times its molar number to obtain the mixed solution of menthyl chloride; according to the molar ratio of magnesium:tetrahydrofuran 1:2 , put magnesium and tetrahydrofuran into a dry three-necked flask equipped with a dropping funnel, a thermometer and a reflux condenser in turn, and then put bromoethane in a molar ratio of magnesium:bromoethane 15:1; Add the above-mentioned menthyl chloride mixture dropwise at a speed of 1 / min. After the dropwise addition, keep the reaction at 80° C. for 2 hours, and cool to room temperature to obtain menthyl magnesium chloride.

[0017] (2) Preparation of Menthyl Chloride

[0018] In the flask that is provided with tail gas absorption device, drop into above-mentioned menthyl magnesium chloride, under the protection of nitrogen, according to the mole ratio of menthyl ...

Embodiment 2

[0022] According to the molar ratio of menthyl chloride:magnesium 1:1, put the menthyl chloride into the tetrahydrofuran of 1 times its molar number to obtain the mixed liquor of menthyl chloride; according to the molar ratio of magnesium:tetrahydrofuran 1:1 , magnesium and tetrahydrofuran were dropped into the flask in turn, and then bromoethane was dropped into the molar ratio of magnesium:bromoethane 10:1; under stirring conditions, the above-mentioned menthyl chloride mixed solution was added dropwise at a speed of 4mL / min , After the dropwise addition, keep the reaction at 50°C for 1h, and cool to room temperature to obtain menthyl magnesium chloride.

[0023] In the flask that is provided with tail gas absorption device, drop into above-mentioned menthyl magnesium chloride, under nitrogen protection, according to the mol ratio of menthyl magnesium chloride: trichloromethyl carbonate 1: 1, under stirring condition, Add trichloromethyl carbonate, heat up to 60°C, react for...

Embodiment 3

[0026] According to the molar ratio of menthyl chloride: magnesium 1: 4, put the menthyl chloride into tetrahydrofuran of 5 times its molar number to obtain the mixed solution of menthyl chloride; according to the molar ratio of magnesium: tetrahydrofuran 1: 5 , magnesium and tetrahydrofuran were dropped into the flask in turn, and then bromoethane was dropped into the molar ratio of magnesium:bromoethane 100:1; under stirring conditions, the above-mentioned menthyl chloride mixed solution was added dropwise at a speed of 12mL / min , After the dropwise addition, keep the reaction at 100°C for 6h, and cool to room temperature to obtain menthyl magnesium chloride.

[0027] In the flask that is provided with tail gas absorption device, drop into above-mentioned menthyl magnesium chloride, under nitrogen protection, according to the mol ratio of menthyl magnesium chloride: trichloromethyl carbonate 1: 4, under stirring condition, Add trichloromethyl carbonate, raise the temperature...

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Abstract

The invention discloses a method for preparing N-ethyl-2-isopropyl-5-methycyclohexane, and belongs to the technical field of amide preparation. The method comprises the following steps: using mint alkyl chloride as a raw material and ethyl bromide as an initiator to firstly prepare chlorinated mint alkyl magnesium; then using trichloromethyl carbonate to prepare mint acyl chloride; and finally obtaining the N-ethyl-2-isopropyl-5-methycyclohexane through the aminolysis reaction of the mint acyl chloride and mono ethyl amine. The method has the advantages of simplicity, simple and convenient operation, mild reaction condition and low production cost; the yield of a product can reach about 80 percent; and the purity of the product reaches more than 99.2 percent. The product prepared by the method has intense cooling flavor effect and long taste retention time, and can be widely applied in the industries of food, medicine, cosmetics, tobacco, and the like.

Description

technical field [0001] The invention belongs to the technical field of amide preparation, in particular to a preparation method of N-ethyl-2-isopropyl-5-methylcyclohexanecarboxamide. technical background [0002] Studies have shown that: menthol amide has a strong cooling effect, long-lasting cooling effect, no bitterness, mild skin feeling, no irritation, no burning feeling, obvious flavoring effect, and can be used well with any cooling agent It can be used in food, medicine, daily chemical, tobacco and other industries, but because of its high price, its scope of application is limited, so the research on the synthesis of menthamide has important economic and social value. [0003] An existing method for preparing N-ethyl-2-isopropyl-5-methylcyclohexanecarboxamide is to start from menthyl chloride and prepare it through steps such as Grignard reaction, acidification, acyl chloride and amidation product. For example, the patent of "High Efficiency Refrigerant--Preparatio...

Claims

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Application Information

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IPC IPC(8): C07C233/58C07C231/02
Inventor 吴永虎王广强朱俊峰柳小平李敏汤文
Owner ANHUI FENGLE PERFUME
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