Synthesis method of isoeugenol

A technology of isoeugenol and synthesis method, which is applied in the direction of isomerization preparation of ether, ether separation/purification, ether preparation, etc., can solve the problems of high content of cis-isoeugenol, environmental pollution of reaction waste liquid, complex production process, etc. , to achieve the effect of simple operation, control of side reactions, and lower distillation temperature

Inactive Publication Date: 2014-06-11
ZIBO VOCATIONAL INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to provide a synthetic method of isoeugenol, aiming to solve the complex production process and high production cost in the current synthetic method of isoeugenol, or the pollution of the environment by reaction waste liquid, or the problem of cis-isoeugenol The problem of too much

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] (1) Grind the dried cloves into clove powder with a particle size diameter of 10 mesh, add 30kg of clove powder to 5L of 1mol / L potassium hydroxide solution and 10L of ethanol, and place it under the condition of 100°C and 24kDz ultrasonic wave for 1h. get decomposition solution;

[0019] (2) Stir and mix the decomposed liquid with toluene at a volume ratio of 5:4, then heat and distill in a vacuum state of 0.09Mpa, control the temperature of the distillation heating place to 50°C, control the temperature of the distillation gas volatilization outlet to 35°C, and distill the distillation gas After being condensed and collected by a condenser, low-boiling point impurities are obtained;

[0020] (3) Continue to heat and distill the remaining filtrate after removing low-boiling impurities in the step (2) in a vacuum state of 0.09Mpa, control the temperature of the distillation heating place to 100°C, control the temperature of the distillation gas volatilization outlet to ...

Embodiment 2

[0022] (1) Grind the dried cloves into clove powder with a particle size diameter of 30 mesh, add 20kg of clove powder to 10L of 1mol / L potassium hydroxide solution and 5L of ethanol, and place it under the condition of 130°C and 28kDz ultrasonic wave for 1h. get decomposition solution;

[0023] (2) Stir and mix the decomposed liquid with a volume ratio of 10:3 and toluene, then heat and distill in a vacuum state of 0.098Mpa, control the temperature of the distillation heating place to 90°C, control the temperature of the distillation gas volatilization outlet to 45°C, and distill The gas is condensed and collected by a condenser to obtain low-boiling point impurities;

[0024] (3) Continue to heat and distill the remaining filtrate after removing low-boiling point impurities in the step (2) in a vacuum state of 0.098Mpa, control the temperature of the distillation heating place to 120°C, control the temperature of the distillation gas volatilization outlet to 105°C, and conve...

Embodiment 3

[0026] (1) Grind the dried cloves into clove powder with a particle size diameter of 20 mesh, add 25kg of clove powder to 8L of 1mol / L potassium hydroxide solution, 10L of ethanol, and place it under the condition of 120°C and 26kDz ultrasonic wave for 1h. get decomposition solution;

[0027] (2) Stir and mix the decomposed liquid with toluene at a volume ratio of 5:2, then heat and distill in a vacuum state of 0.09Mpa, control the temperature of the distillation heating place to 60°C, control the temperature of the distillation gas volatilization outlet to 40°C, and distill the distillation gas Obtain low-boiling point impurities after being condensed and collected with a condenser; Wherein, the volume ratio of the decomposed liquid and toluene is;

[0028] (3) Continue to heat and distill the remaining filtrate after removing low-boiling point impurities in the step (2) in a vacuum state of 0.098Mpa, control the temperature of the distillation heating place to 120°C, control...

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Abstract

The invention provides a synthesis method of isoeugenol. The method comprises the following steps: adding ground cloves powder to a potassium hydroxide solution which is 1mol/L in concentration and ethanol, and keeping under an ultrasonic condition at 100-130 DEG C for 1-2 hours to obtain a decomposition solution; stirring and mixing the decomposition solution with methylbenzene, heating and distilling under a vacuum state, controlling distilling and heating temperature at 50-90 DEG C, controlling temperature of a distillation gas volatilization outlet at 35-45 DEG C, and condensing and collecting distillation gas through a condenser to obtain low boiling point impurities; continuing to distill rest filtrate after removing the low boiling point impurities, controlling distilling and heating temperature at 100-120 DEG C, controlling temperature of the distillation gas volatilization outlet at 90-105 DEG C, and condensing and collecting the distillation gas through the condenser to obtain the isoeugenol. The synthesis method disclosed by the invention is light in environmental pollution, more simple to operate and quite low in production cost; moreover, content of trans-isoeugenol can achieve more than 95% in the isoeugenol.

Description

technical field [0001] The invention belongs to the field of compound synthesis, in particular to a method for synthesizing isoeugenol. Background technique [0002] Isoeugenol (4-propenyl-2-methoxyphenol, molecular formula C10H 12 o 2 ) is a light yellow slightly thick liquid, insoluble in water and glycerin, soluble in organic solvents such as ethanol; it has a soft, sweet and clear spicy fragrance, such as carnation and clove; it is mainly used to prepare essence and vanillin, and can be used in Prepare essential oils such as ylang-ylang and nutmeg; it can also be used to prepare food flavors with raspberry, peach, spicy and clove flavors; it is also a raw material for semi-synthetic vanillin. The structure of isoeugenol exists in two forms: cis and mode, but because cis isoeugenol has certain toxicity, when it is used as a commodity, it is generally required that the proportion of cis in the cis-trans mixture should not exceed 10%. At present, the synthesis methods of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/23C07C41/32
CPCC07C41/32C07C41/34C07C43/23
Inventor 张淑新
Owner ZIBO VOCATIONAL INST
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