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Method for preparing high-content helional

A new technology of jasmonal and high content, which is applied in the field of organic synthesis of spices, can solve the problems of difficult recovery of catalysts, difficult separation of products, and reduced yield, so as to achieve easy purification, avoid restrictions on raw material sources, and reduce waste Effect

Active Publication Date: 2014-12-17
安徽华业香料合肥有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation method of Xinyangjasmonal in the prior art generally focuses on solving the problem that the product is not easy to separate after the reaction, the catalyst is difficult to recycle, and it is very easy to cause environmental pollution. The by-products of jasmonol and jasmonic acid reduce the yield and are difficult to separate. The new jasmonal has many impurities, so it cannot effectively keep the fragrance of the new jasmonal lasting and pure.

Method used

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  • Method for preparing high-content helional

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Experimental program
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Effect test

Embodiment 1

[0025] ingredients

[0026] a. First add 300kg of pepper ring and 10kg of boron trifluoride into the first high-level tank 3, and send the mixed material from the first high-level tank 3 into the enamel reaction kettle 4 by vacuum suction. After the feeding is completed , feed nitrogen to replace the vacuum of the enamel reactor 4, add 0.8 kg of butyl hydroxyanisole from the hand hole of the enamel reactor 4, start the mixer and mix evenly.

[0027] b. Prepare the dropwise mixture in stirring pot 1, first add 200 kg of pepper ring, then add 200 kg of 2-methallyl diacetate, start the mixer and mix well.

[0028] Alkylation reaction

[0029] c. Turn on the frozen water to lower the temperature of the enamel reaction kettle 4. When the temperature of the kettle is lower than 10°C, start to drop the mixture of piperonylcycline and 2-methylallyl diacetate through the dripping pump 2 under normal pressure. , the kettle temperature was controlled at 10°C by adjusting the chilled wa...

Embodiment 2

[0039] ingredients

[0040] a. First add 320 kg of pepper ring and 10.5 kg of boron trifluoride into the first high-level tank 3, and send the mixed material from the first high-level tank 3 into the enamel reaction kettle 4 by means of vacuum suction. After the feeding is completed, Nitrogen was introduced to replace the vacuum of the enamel reactor 4, and 0.8 kg of a mixture of butyl hydroxyanisole, dibutyl hydroxytoluene and propyl gallate was added from the hand hole of the enamel reactor 4, and the mixer was started to mix evenly.

[0041] b. Prepare the dropwise mixture in the stirring pot 1, first add 220 kg of pepper ring, then add 220 kg of 2-methallyl diacetate, start the mixer and mix well.

[0042] Alkylation reaction

[0043] c. Turn on the frozen water to lower the temperature of the enamel reaction kettle 4. When the temperature of the kettle is lower than 10°C, start to drop the mixture of piperonylcycline and 2-methylallyl diacetate through the dripping pump ...

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Abstract

The invention discloses a method for preparing high-content helional. The method comprises the following steps: adding benzodioxole and boron trifluoride into an enameled reaction kettle, and adding an oil-soluble antioxidant into the enameled reaction kettle; adding the benzodioxole into an agitating pan, adding 2-methylallyl diacetate to prepare and drip the mixture; dripping the mixture at the kettle temperature of less than 10 DEG C for 4-10 hours; transferring the reaction products into a distillation still, recovering the benzodioxole, and distilling the helional monoester; adding methanol, water and potassium hydroxide into the reaction kettle, adding the helional monoester, maintaining the temperature of 50-90 DEG C, carrying out a hydrolysis reaction, cooling within 3-5 hours, ending the reaction, transferring to a washing pot, standing for 30 minutes, and separating the lower water; and transferring the reaction products in the washing pot into a fractionation kettle, recovering the methanol at normal pressure, and performing fractionation on the crude helional to obtain the finished product with the high content of 98.5 weight percent. The method is mild in reaction conditions, convenient to operate, readily available in raw materials and low in cost.

Description

technical field [0001] The invention relates to a method for preparing organic synthetic perfume, in particular to a method for preparing high-content Xinyangjasmonal. Background technique [0002] Xinyang jasmonal is a preparation spice with an ozone-like top note of flowers. It not only has the gentle fragrance of fresh flowers and grasses such as rabbit ear oxalin, lilac, fresh mowed grass and cyclamen, but also fresh melon and watermelon. This kind of fruity green fragrance can be used to blend almost all floral fragrances such as cyclamen, jasmine and rose. It is used in the deployment of various high-end perfumes, cosmetics, deodorants, liquid detergents, and soap essences, and the dosage can reach 10%. It is used in conjunction with methyl dihydrojasmonate, and the effect is excellent. It is internationally famous Famous brand perfumes such as "Eau Sauvage" and "Diorella" produced by the "Dior" factory in Beijing have added Xinyang Jasmine. Xinyang jasmonal is an in...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D317/54
Inventor 王天义范一义汪洋汪民富董金龙
Owner 安徽华业香料合肥有限公司
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