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Synthetic method for macrocyclic musk ketone

A synthetic method and technology of muskone, applied in chemical instruments and methods, preparation of carbon-based compounds, preparation of organic compounds, etc., can solve the problems of no synthetic fragrance cyclopentadecanone, etc., prevent cranial neurasthenia, improve active and effective

Inactive Publication Date: 2017-02-15
昆明酷特利生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] At present, there is no report on the method of synthesizing spice cyclopentadecanone from garlic fruit oil in the prior art

Method used

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  • Synthetic method for macrocyclic musk ketone
  • Synthetic method for macrocyclic musk ketone
  • Synthetic method for macrocyclic musk ketone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] 1. Preparation and purification of tetracos-15-enoic acid.

[0031] 1.1 Extraction of garlic fruit oil:

[0032]Garlic nuts are finely ground in a mortar, wrapped with filter paper, put into a Soxhlet extractor, and extracted with petroleum ether as a solvent under reflux for 6 hours. The extracted garlic oil is evaporated to dryness and stored for later use.

[0033] 1.2 Preparation and purification of tetracos-15-enoic acid.

[0034] 1.2.1 Saponification and acidification of garlic fruit oil:

[0035] Add NaOH to denatured alcohol and stir to dissolve. After the dissolution is complete, add it to a container containing garlic fruit oil, stir and saponify in the electric heating mantle for 4 hours; Wash with hot water several times to obtain mixed fatty acids for later use.

[0036] 1.2.2 Tetracos-15-enoic acid recrystallization:

[0037] Using absolute ethanol, acetone, and pyridine as a single solvent, carry out recrystallization, and detect the purity by gas pha...

Embodiment 2

[0097] Synthesis of cyclopentadecanone (macrocyclic muscone).

[0098] Experimental route (see figure 1 ): Tetracos-15-enoic acid ozonation method.

[0099] resolve resolution:

[0100] First prepare tetracos-15-enoic acid:

[0101] 1. Preparation and purification of tetracos-15-enoic acid.

[0102] 1.1 Extraction of garlic fruit oil:

[0103] Garlic nuts are finely ground in a mortar, wrapped with filter paper, put into a Soxhlet extractor, and extracted with petroleum ether as a solvent under reflux for 6 hours. The extracted garlic oil is evaporated to dryness and stored for later use.

[0104] 1.2 Preparation and purification of tetracos-15-enoic acid.

[0105] 1.2.1 Saponification and acidification of garlic fruit oil:

[0106] Add NaOH to denatured alcohol and stir to dissolve. After the dissolution is complete, add it to a container containing garlic fruit oil, stir and saponify in the electric heating mantle for 4 hours; Wash with hot water several times to obtain...

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Abstract

The invention provides a method for synthesizing high-grade perfume, i.e., high-value musk perfume cyclopentadecanone (macrocyclic musk ketone), from Malania oleifera oil. The Malania oleifera oil is used as a raw material and subjected to saponification, acidification, recrystallization, ozonization, oxidation, esterification, cyclization and reduction successively so as to prepare cyclopentadecanone. The method is high in yield, good in benefits and low in cost and overcomes the shortcomings of complex production process, low yield, high cost and no market advantage in the prior art. The Malania oleifera oil contains 40 to 60% of tetracos-15-enoic acid which is an ideal raw material for synthesis of the high-value musk perfume. Tetracos-15-enoic acid is a necessary nutriment for development of the brain, exerts critical effect on improvement of the activity of cranial nerves and prevention of encephalasthenia, has good curative effect on cardiovascular diseases and diseases caused by autoimmune deficiency, and can be used as a medicine and a health product.

Description

[0001] Technical field: [0002] The invention belongs to the technical field of chemical products, and specifically relates to a method for synthesizing additives for medicine, health products and cosmetics, and more specifically, relates to a method for synthesizing macrocyclic muscone from garlic fruit oil. [0003] Background technique: [0004] Musk is a precious animal spice. As early as the Eastern Han Dynasty, musk was known as the king of spices. It has strong diffusivity and inducing power, has a special soft and elegant aroma, good fragrance-increasing effect and excellent fragrance-fixing ability. It is an indispensable fixative in the deployment of high-end fragrances and is widely used in flavors and fragrances Industry, tobacco industry, food industry, daily chemical industry and other industries. In the blending of flavors and fragrances, as long as one ten-thousandth of musk is added, not only can the essence and perfuming products have an elegant musk aroma, ...

Claims

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Application Information

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IPC IPC(8): C07C45/61C07C49/385
CPCC07C45/61C07C45/41C07C51/34C07C51/487C07C67/08C07C49/385C07C49/487C07C69/34C07C55/02C07C57/03
Inventor 杨宇明王娟刘祥义施蕊陈汓
Owner 昆明酷特利生物科技有限公司
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