Method for preparing mint-based carboxylic acid in process of synthesizing N-Ethyl-p-menthane-3-carboxamide
A technology of menthyl amide and charge-based carboxylic acid, which is applied in the field of preparation of menthyl carboxylic acid in the process of synthesizing menthyl amide, can solve the problems of complex process, long production cycle, low product yield, etc., and achieves reduction of raw material consumption and improvement of products. Yield, the effect of shortening the reaction time
Inactive Publication Date: 2010-03-03
HENAN HUALONG SPICE
View PDF0 Cites 8 Cited by
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Another kind of method is to use natural menthol as raw material, through chlorination, then through Grignard reagent carboxylation reaction and amidation reaction etc., make menthyl amide (WS-3) cooling agent, this traditional method complex process, production cycle long, low product yield
Method used
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View moreImage
Smart Image Click on the blue labels to locate them in the text.
Smart ImageViewing Examples
Examples
Experimental program
Comparison scheme
Effect test
Embodiment Construction
[0009] The preparation method of menthyl carboxylic acid in the process of synthesizing menthyl amide is to select natural menthol as raw material, through chlorination reaction, then through Grignard reagent carboxylation reaction and amidation reaction, etc. to prepare menthyl amide (WS-3) cooling agent Synthetic method, focusing on the preparation technology of menthyl carboxylic acid in the process of synthesizing menthyl amide. In a 1 liter stainless steel pressure reaction kettle equipped with a stirrer, thermometer, pressure gauge and condensing reflux device, add metal magnesium chips, tetrahydrofuran and toluene, heat with an electric heating mantle to make the temperature in the kettle reach about 80 degrees, and stir slowly Slowly add the menthyl chloride produced by the chlorination of natural menthol. After the menthyl chloride is added dropwise and the reflux is stable, the carbon dioxide cylinder is passed into the pressure reactor in a closed state to adjust the...
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More PUM
Login to View More Abstract
The invention provides a method for preparing mint-based carboxylic acid in a process of synthesizing N-Ethyl-p-menthane-3-carboxamide. Metal magnesium chips, tetrahydrofuran and methylbenzene are added in a stainless steel pressure reaction kettle with the volume of 1L, which is internally provided with a mixer, a thermometer and a reflux condensation device; the kettle is heated to be about 80 DEG C; under a mixing condition, the mint-based chlorine made of natural menthol is dropped slowly; carbon dioxide is introduced in the pressure reaction kettle under a sealed state; the flow rate of the carbon dioxide is adjusted, the pressure of the reaction kettle is kept at about 0.5MPa; the reaction time is kept about 10 hours; the reactants are acidified and washed by 30% of hydrochloric acid; the mint-based carboxylic acid is obtained after recovering the solvent; 85g of mint-based carboxylic acid is obtained by weighing; by gas chromatography, the content of the mint-based carboxylic acid is 87.5% (levo form); the mint-based carboxylic acid reacts with the thionyl chloride to obtain the mint-based acyl chloride; the mint-based acyl chloride reacts with ethylamine solution (70%); theN-Ethyl-p-menthane-3-carboxamide (WS-3) cool flavorings are obtained by rectifying, crystallizing, pumping and filtrating and drying; and 52g of N-Ethyl-p-menthane-3-carboxamide (WS-3) is obtained byweighing.
Description
1. Technical field: [0001] The invention relates to the technical field of preparation of menthyl amide (WS-3) cooling agent, in particular to a preparation method of menthyl carboxylic acid in the process of synthesizing menthyl amide. 2. Background technology: [0002] Menthamide (WS-3) cooling agent, its chemical name is N-ethyl-5-methyl-3-isopropyl-cyclohexylamide, and its molecular formula is C 13 h 25 NO, CAS 39711-79-0, FEMA 3455, has a light mint aroma, is a fresh and long-lasting cool taste with strong impact, can be used in conjunction with other cooling agents, and can be directly used in food, medicine and daily use In chemical products, it can be widely used in the preparation of food flavors such as chewing gum, fructose, ice cream, etc., it can be used in the preparation of daily chemical flavors such as toothpaste, toiletries, cosmetics, air fresheners, tobacco, etc., and it can also be used in medicine, insect repellent Agents, etc. Menthylamide (WS-3) has...
Claims
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More Application Information
Patent Timeline
Login to View More Patent Type & Authority Applications(China)
IPC IPC(8): C07C233/58C07C231/02C07C61/08C07C51/15
Inventor 王宝玉陈恩治王慧晨
Owner HENAN HUALONG SPICE