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Method for preparing beta-damascone by utilizing beta-ionone

A technology of ionone and damascenone, which is applied in the preparation of carbon-based compounds, chemical instruments and methods, preparation of hydroxyl compounds, etc., can solve the problems of low yield of β-damascenone, etc., and achieves simple operation and flexible and controllable conditions. Effect

Inactive Publication Date: 2017-12-22
王显权
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention aims at the above-mentioned existing technical problems, and provides a method for preparing β-damascenone by using β-ionone, so as to solve the technical problem of low acquisition rate of β-damascenone prepared by the existing process

Method used

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  • Method for preparing beta-damascone by utilizing beta-ionone
  • Method for preparing beta-damascone by utilizing beta-ionone
  • Method for preparing beta-damascone by utilizing beta-ionone

Examples

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Effect test

Embodiment 1

[0024] Embodiment 1: utilize β-ionone to prepare the method for β-damascenone, comprise the following steps:

[0025] Step 1. Oxidation: add β-ionone into the enamel reaction kettle, heat after stirring, add peracetic acid dropwise at 40°C, and maintain it at this temperature for 4 hours; the oxygen content of the peracetic acid is 10% excessive; Add 10% soda ash, neutralize to pH 8, hydrolyze for 1 hour, add 40% sodium bisulfite, heat to 40°C, and stir for 3 hours;

[0026] Step 2, distilling hydroxyacetone at 40°C and 1.6kPa; the remaining material obtained after recovering hydroxyacetone is retained for subsequent use;

[0027] Step 3. Decomposition: Keep the remaining material temperature at 40°C, add soda ash while stirring, then put it into a separator, let it stand for stratification, take the upper layer of oil, put it in a reaction kettle for vacuum distillation, collect 70°C, 0.4 fraction of kpa;

[0028] Step 4: Add β-citral ether solution to the reaction kettle, ...

Embodiment 2

[0031] Embodiment 2: utilize β-ionone to prepare the method for β-damascenone, comprise the following steps:

[0032] Step 1. Oxidation: Add β-ionone into the enamel reaction kettle, heat after stirring, add peracetic acid dropwise at 40°C, and maintain it at this temperature for 3 hours; the oxygen content of the peracetic acid is 10% excessive; Add 10% soda ash, neutralize to pH 8, hydrolyze for 2 hours, add 40% sodium bisulfite, heat to 40°C, and stir for 2 hours;

[0033] Step 2, distilling hydroxyacetone at 43°C and 1.6kPa; the remaining material obtained after recovering hydroxyacetone is kept for later use;

[0034] Step 3. Decomposition: Keep the remaining material temperature at 40°C, add soda ash while stirring, then put it into a separator, let it stand for stratification, take the upper layer of oil, put it in a reaction kettle for vacuum distillation, collect at 60°C, 0.22 fraction of kpa;

[0035] Step 4: Add β-citral ether solution into the reaction kettle, st...

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Abstract

The invention discloses a method for preparing beta-damascone by utilizing beta-ionone, and belongs to the technical field of chemical synthesis. The method comprises the following steps: adding the beta-ionone, peracetic acid, 10% sodium carbonate, and 40% sodium bisulfite into a reaction kettle; adding sodium carbonate under a temperature condition of 40 DEG C, allowing the mixed materials to stand for layering, collecting the upper-layer oil liquid, placing the upper-layer oil liquid into a reaction kettle, performing reduced-pressure distillation, and collecting a fraction at 60-70 DEG C and 0.4-0.22kpa; adding a beta-citral ethyl ether liquid into the reaction kettle, performing cooling, performing heating to 15-20 DEG C, adding allylmagnesium bromide, an ethyl ether liquid and 10% ammonium chloride, performing hydrolysis under a temperature of 30 DEG C under stirring, allowing the obtained materials to stand, and collecting an upper-layer oil liquid; performing distillation on the oil liquid under a vacuum condition, and collecting a fraction at 75-80 DEG C and 0.26kpa; adding a concentrated alcohol pyridine liquid and pyridinium chlorochromate(Pcc) powder into the fraction, filtering out chromic oxide generated by the reaction, adding water, and performing washing; merging the filtrate and the wash liquid, and adding 10% NaOH; and adding an aminourea liquid into the oil liquid, transferring a mixed liquid to a separator, allowing the mixed liquid to stand for layering, and collecting the low-layer aqueous solution to obtain the beta-damascone. According to the invention, the yield of the beta-damascone obtained by the method can achieve 84% or more.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a method for preparing β-damascenone by using β-ionone. Background technique [0002] β-ionone is a light yellow to yellow oily liquid with a characteristic aroma at room temperature, so it is an extremely important spice, mostly used in soap flavors and perfumes, and is also a raw material for the synthesis of vitamin A. [0003] β-Damascenone, also known as β-Turkelenone, is a light yellow transparent liquid. β-Damascenone is a trace key aroma component discovered by Ohloff, a famous fragrance chemist, in Bulgarian Turkic rose essential oil in the 1960s. Its content in flower essential oil is generally only 0.05%, but it is the most It is an important aroma component. In addition, this component is also widely found in cabbage, tobacco leaves, black tea, apples and other foods. It is a precious and safe spice. Just because β-Damascenone has a strong rose aroma, ful...

Claims

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Application Information

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IPC IPC(8): C07C45/29C07C49/557
CPCC07C29/40C07C45/292C07C45/42C07C49/557C07C33/14C07C47/42
Inventor 王显权
Owner 王显权
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