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CN-122010756-A - Preparation method, atomization liquid and atomization device of N- (2-methylcyclohexyl) -2,3,4,5, 6-pentafluorobenzamide

CN122010756ACN 122010756 ACN122010756 ACN 122010756ACN-122010756-A

Abstract

The embodiment of the application provides a preparation method, an atomization liquid and an atomization device of N- (2-methylcyclohexyl) -2,3,4,5, 6-pentafluorobenzamide, which can generate a target product crude product of N- (2-methylcyclohexyl) -2,3,4,5, 6-pentafluorobenzamide through the synthesis reaction of pentafluorobenzoic acid and 2-methylcyclohexylamine in an organic solvent under the action of an alkaline substance and a condensing agent, filter the target product in a second mixed liquid, dissolve the second mixed liquid in ethanol, decolorize the second mixed liquid by using active carbon, add water into a filtrate to separate out solids after the thermal filtration, filter the solids, and dry filter residues to obtain N- (2-methylcyclohexyl) -2,3,4,5, 6-pentafluorobenzamide with the purity of more than or equal to 99%, so that the problem that the prior art cannot effectively synthesize high-purity N- (2-methylcyclohexyl) -2,3,4,5, 6-pentafluorobenzamide can be effectively solved.

Inventors

  • PENG JINAN
  • DONG ZEYI
  • CHEN ZHICHAO
  • HE CHAO
  • FU YAO

Assignees

  • 爱奇迹创造有限公司

Dates

Publication Date
20260512
Application Date
20251218

Claims (10)

  1. 1. A process for the preparation of N- (2-methylcyclohexyl) -2,3,4,5, 6-pentafluorobenzamide, comprising: Adding pentafluorobenzoic acid, an alkaline substance and 2-methylcyclohexylamine into an organic solvent to obtain a first mixed solution; adding a condensing agent into the first mixed solution, and performing condensation reaction to obtain a crude product of a target product; Adding the crude product of the target product into a second mixed solution for filtering to obtain a first purified product; Dissolving the first purified matter in ethanol, decolorizing with active carbon, performing hot filtration to obtain filtrate, adding water into the filtrate to precipitate solid, filtering to obtain filter residue, and drying the filter residue to obtain N- (2-methylcyclohexyl) -2,3,4,5, 6-pentafluorobenzamide, wherein the purity of the N- (2-methylcyclohexyl) -2,3,4,5, 6-pentafluorobenzamide is greater than or equal to 99%.
  2. 2. The process according to claim 1, wherein the basic substance comprises at least one of triethylamine, N-diisopropylethylamine, sodium hydrogencarbonate, potassium carbonate, sodium carbonate, and/or The condensing agent comprises at least one of N, N, N ', N' -tetramethyl-O- (7-azabenzotriazol-1-yl) hexafluorophosphate, benzotriazole-N, N, N ', N' -tetramethyl urea hexafluorophosphate, a calt condensing agent, 1H-benzotriazole-1-yl oxygen tripyrrolidinyl hexafluorophosphate, and/or The organic solvent comprises at least one of ethyl acetate, dichloromethane, acetonitrile, tetrahydrofuran and N, N-dimethylformamide.
  3. 3. The process according to claim 1, wherein the molar ratio of pentafluorobenzoic acid to 2-methylcyclohexylamine in the first mixed solution is 1 (1-1.2), and/or The molar ratio of the pentafluorobenzoic acid to the condensing agent is 1 (1-1.2), and/or The molar ratio of the pentafluorobenzoic acid to the alkaline substance is 1 (1.2-1.5).
  4. 4. The method according to claim 1, wherein the ratio between the amount of the substance of pentafluorobenzoic acid and the volume of the organic solvent in the first mixed solution is 1/8~1/3mol/mL.
  5. 5. The method according to claim 1, wherein the condensation reaction is carried out to obtain a crude product of the objective product, comprising: Washing the reaction product of the condensation reaction with water to obtain a washing liquid, and sequentially carrying out extraction treatment, drying treatment and reduced pressure concentration treatment on the washing liquid to obtain the crude product of the target product.
  6. 6. The process according to claim 5, wherein the extractant in the extraction comprises ethyl acetate and/or The drying treatment adopts a drying agent for drying, and the drying agent comprises at least one of anhydrous Na 2 SO 4 and anhydrous magnesium sulfate.
  7. 7. The method according to any one of claims 1 to 6, wherein the second mixed solution comprises ethyl acetate and petroleum ether.
  8. 8. The preparation method of claim 7, wherein the volume ratio of ethyl acetate to petroleum ether in the second mixed solution is 1 (5-10).
  9. 9. An atomized liquid comprising an active substance and a sweetener, wherein the sweetener comprises N- (2-methylcyclohexyl) -2,3,4,5, 6-pentafluorobenzamide prepared by the method according to any one of claims 1 to 8.
  10. 10. An atomizer comprising an atomizer having the atomized liquid of claim 9 stored in a reservoir of the atomizer.

Description

Preparation method, atomization liquid and atomization device of N- (2-methylcyclohexyl) -2,3,4,5, 6-pentafluorobenzamide Technical Field The application belongs to the technical field of sweeteners, and particularly relates to a preparation method, an atomization liquid and an atomization device of N- (2-methylcyclohexyl) -2,3,4,5, 6-pentafluorobenzamide. Background An electronic atomizing device is a device that atomizes an atomized liquid into an aerosol by means of heating or the like. The sweetener is an important component of the atomized liquid, so that the taste can be optimized, and the use experience of consumers is improved. Currently, sweeteners which are important components of the atomized liquid mainly include neotame, sucralose, neohesperidin dihydrochalcone (NHDC), stevioside (GSG), and the like. The sweetener is developed by taking food and beverage as application scenes, and has obvious defects in application in an electronic atomization device. For example, neotame is prone to breakdown and bitter, sucralose and NHDC are prone to core sticking, etc. N- (2-methylcyclohexyl) -2,3,4,5, 6-pentafluorobenzamide is used as an artificial synthetic sweetener, and the N- (2-methylcyclohexyl) -2,3,4,5, 6-pentafluorobenzamide obtained by the existing preparation method has low purity, large potential safety hazard, high energy consumption and high cost. Disclosure of Invention The application aims to solve the technical problem of providing a preparation method, an atomization liquid and an atomization device of N- (2-methylcyclohexyl) -2,3,4,5, 6-pentafluorobenzamide so as to solve the problem that the prior art cannot effectively synthesize high-purity N- (2-methylcyclohexyl) -2,3,4,5, 6-pentafluorobenzamide. In order to solve the problems, the application is realized by the following technical scheme: the application provides a preparation method of N- (2-methylcyclohexyl) -2,3,4,5, 6-pentafluorobenzamide, which comprises the following steps: Adding pentafluorobenzoic acid, an alkaline substance and 2-methylcyclohexylamine into an organic solvent to obtain a first mixed solution; adding a condensing agent into the first mixed solution, and performing condensation reaction to obtain a crude product of a target product; Adding the crude product of the target product into a second mixed solution for filtering to obtain a first purified product; Dissolving the first purified matter in ethanol, decolorizing with active carbon, performing hot filtration to obtain filtrate, adding water into the filtrate to precipitate solid, filtering to obtain filter residue, and drying the filter residue to obtain N- (2-methylcyclohexyl) -2,3,4,5, 6-pentafluorobenzamide, wherein the purity of the N- (2-methylcyclohexyl) -2,3,4,5, 6-pentafluorobenzamide is greater than or equal to 99%. Further, in the preparation method, the alkaline substance comprises at least one of triethylamine, N-diisopropylethylamine, sodium bicarbonate, potassium carbonate and sodium carbonate, and/or The condensing agent comprises at least one of N, N, N ', N' -tetramethyl-O- (7-azabenzotriazol-1-yl) hexafluorophosphate, benzotriazole-N, N, N ', N' -tetramethyl urea hexafluorophosphate, a calt condensing agent, 1H-benzotriazole-1-yl oxygen tripyrrolidinyl hexafluorophosphate, and/or The organic solvent comprises at least one of ethyl acetate, dichloromethane, acetonitrile, tetrahydrofuran and N, N-dimethylformamide. Further, in the first mixed solution, the molar ratio of the pentafluorobenzoic acid to the 2-methylcyclohexylamine is 1 (1-1.2), and/or The molar ratio of the pentafluorobenzoic acid to the condensing agent is 1 (1-1.2), and/or The molar ratio of the pentafluorobenzoic acid to the alkaline substance is 1 (1.2-1.5). Further, in the preparation method, the ratio of the amount (mol) of the substance of pentafluorobenzoic acid to the volume (mL) of the organic solvent in the first mixed solution is 1/8~1/3mol/mL. Further, in the preparation method, the condensation reaction is performed to obtain a crude product of the target product, which comprises the following steps: Washing the reaction product of the condensation reaction with water to obtain a washing liquid, and sequentially carrying out extraction treatment, drying treatment and reduced pressure concentration treatment on the washing liquid to obtain the crude product of the target product. Further, in the preparation method, the extractant in the extraction treatment comprises ethyl acetate, and/or The drying treatment adopts a drying agent for drying, and the drying agent comprises at least one of anhydrous Na 2SO4 and anhydrous magnesium sulfate. Further, in the preparation method, the second mixed solution comprises ethyl acetate and petroleum ether. In the preparation method, the volume ratio of the ethyl acetate to the petroleum ether in the second mixed solution is 1 (5-10). The application also provides an atomized liquid which comprises an active substance and a swe