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Method for synthesizing arbordinone

A technology of cedaranone and a synthesis method is applied in chemical instruments and methods, oxidation preparation of carbonyl compounds, organic compounds/hydrides/coordination complex catalysts, etc., and can solve the problems such as not being well utilized of cypressene, and the like, To achieve the effect of easy regeneration and recycling, good application prospect and long fragrance retention time

Active Publication Date: 2020-08-07
NANJING FORESTRY UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Both α, β-cedrene and pagodarene are derived from cedarwood oil, but comparatively speaking, α-cedrene and β-cedrene have been studied more in the synthesis of high-end cedarwood fragrances, while pagodarene has not been well studied easy to use

Method used

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  • Method for synthesizing arbordinone
  • Method for synthesizing arbordinone
  • Method for synthesizing arbordinone

Examples

Experimental program
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Embodiment 1

[0030] A kind of synthetic method of phoenix cypress, comprising the following steps:

[0031] (1) Synthesis of activated carbon-supported quaternary ammonium phosphotungstic acid: add 40mL 1,2-dichloroethane and 5.76g phosphotungstic acid into the reactor, stir well to dissolve; then weigh 1.96g hexadecyl Dissolve trimethylammonium chloride in 20mL 1,2-dichloroethane solution, slowly drop it into the reactor, and keep stirring; after the dropwise addition, continue stirring at 40°C for 2h, the reaction is over; the reaction solution is cooled to room temperature, let stand for 1 hour, and then filter under reduced pressure; the solid was washed with distilled water, and dried at 80°C for 8 hours to obtain a white solid powder, that is, quaternary ammonium phosphotungstic acid; weigh 1g of pretreated activated carbon, 0.2g of phosphotungstic acid After stirring quaternary ammonium salt and 20mL distilled water at room temperature for 6 hours, filter under reduced pressure, put...

Embodiment 2

[0035] A kind of synthetic method of phoenix cypress, comprising the following steps:

[0036] (1) Synthesis of activated carbon-supported quaternary ammonium phosphotungstic acid: add 40mL 30% H to the reactor 2 o 2 and 5.76g phosphotungstic acid, fully stirred to dissolve; then weighed 1.96g hexadecyltrimethylammonium chloride and dissolved in 20mL 30% H 2 o 2 solution, slowly drop it into the reactor, and keep stirring; after the dropwise addition, continue to stir at 40°C for 2h, the reaction is over; the reaction solution is cooled to room temperature, and after standing for 1h, it is filtered under reduced pressure; the solid is washed with distilled water , dried at 80°C for 8 hours to obtain a white solid powder, quaternary ammonium phosphotungstic acid; weigh 1 g of pretreated activated carbon, 0.3 g of quaternary ammonium phosphotungstic acid and 20 mL of distilled water, stir at room temperature for 6 hours, and filter under reduced pressure , the filter cake was...

Embodiment 3

[0040] A kind of synthetic method of phoenix cypress, comprising the following steps:

[0041](1) Synthesis of activated carbon-supported quaternary ammonium phosphotungstic acid: add 40mL of absolute ethanol and 5.76g of phosphotungstic acid into the reactor, stir well to dissolve; then weigh 1.96g of hexadecyl trimethyl chloride Dissolve ammonium in 20mL of absolute ethanol solution, slowly drop it into the reactor, and keep stirring; after the dropwise addition, continue stirring at 40°C for 2h, and the reaction ends; filter; the solid was washed with distilled water, and dried at 80°C for 8 hours to obtain a white solid powder, quaternary ammonium phosphotungstic acid; weigh 1 g of pretreated activated carbon, 0.4 g of quaternary ammonium phosphotungstic acid and 20 mL of distilled water, and After stirring for 6 hours, filter under reduced pressure, put the filter cake washed with distilled water into an oven, and dry at 80°C for 8 hours to obtain a quaternary ammonium ph...

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Abstract

The invention discloses a method for synthesizing arbordinone, and belongs to the technical field of fine organic chemical synthesis. The method comprises the following steps: taking phosphotungstic acid and hexadecyl trimethyl ammonium chloride as raw materials to prepare phosphotungstic acid quaternary ammonium salt, and loading the phosphotungstic acid quaternary ammonium salt on activated carbon to prepare an activated carbon loaded phosphotungstic acid quaternary ammonium salt catalyst; under the action of an activated carbon loaded phosphotungstic acid quaternary ammonium salt catalyst,carrying out oxidation reaction on the cedar wood alkene to obtain cedar wood alkanone, wherein the molecular formula of the cedar wood alkyl ketone is C15H24O. Activated carbon loaded phosphotungsticacid quaternary ammonium salt is used as a catalyst, stability of catalysts can be enhanced, the method facilitates regeneration and recycling of the catalyst, reduces emission of waste materials, isbeneficial to the environment, is simple in synthesis method, small in corrosion to equipment, safe and environmentally friendly, and the prepared Luohania hancei alkyl ketone has the smell of elecampane and ambergris, is noble in fragrance, long in fragrance lasting time and high in stability, and has a good application prospect.

Description

technical field [0001] The invention belongs to the technical field of synthesis of fine organic chemicals, and in particular relates to a method for synthesizing luohancypressanone. Background technique [0002] Cedarwood ketones are important monomeric fragrances, which are colorless to pale yellow oily liquids with woody and ambergris aromas. The aroma is valuable and long-lasting. It can also be used in the preparation of perfume, leather and tobacco. Similar products of cedrene are mainly oxidatively synthesized from α, β- cedrene as raw material, while the synthesis of cedrene from phoenix has not yet been studied in China, and there are relatively few related studies abroad. Phthalic acid oxidation, peracetic acid oxidation, m-chloroperoxybenzoic acid oxidation and other methods. Organic peroxyacids are highly corrosive, unstable in nature, easy to decompose when exposed to heat, heavy metal ions, strong alkali, etc., and are subject to certain restrictions in use. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/28C07C49/453B01J31/02B01J27/188
CPCB01J27/188B01J31/0239B01J2231/70C07C45/28C07C49/453C07C2603/96Y02P20/584
Inventor 朱凯张胜
Owner NANJING FORESTRY UNIV
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