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Preparation method of industrial musk tonalide

An industrial technology of musk tona, which is applied in the direction of condensation preparation of carbonyl compounds, organic chemistry, etc., can solve the problems of human skin damage, rising demand and high production cost, and achieves the effects of low production cost, mild conditions and high yield.

Inactive Publication Date: 2013-10-30
HENAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Tuna musk (7-acetyl-1,1,3,4,4,6-hexamethyltetrahydronaphthalene) is a daily-use fragrance, Tuna musk belongs to the bicyclic tetralin musk, with a strong Powder scent, excellent quality, elegant aroma, long-lasting fragrance, giving people a very comfortable and pleasant feeling, the product has strong diffusivity, good coordination, stable in acid-base medium, not easy to change color, strong adhesion to fibers , suitable for high-end cosmetics such as soaps and face powders, as well as detergents and fabric softeners. This product is internationally recognized as a very ideal fragrance that is safe to use and harmless to human skin. The development and research of nitro musk is still in its infancy, and it still needs to be imported from abroad. At present, nitro musk is often used in the domestic market, but nitro musk has serious damage to human skin, causing skin cancer, and has become a prohibited product. Then become the ideal substitute of nitromusk, according to relevant display, we can know that the domestic demand of musk for breathing is rising sharply, and the method yield of musk for synthesizing is low at present, and purity is low, and cost is expensive, and production cost height, takes a long time

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Step 1, preparation of intermediate 1,1,3,4,4,6-hexamethyltetralin

[0024] 1) Take 2 moles of p-cymene, 1 mole of 2,3-dimethyl-1-butene and 1.05 moles of tert-butyl chloride according to the molecular mass ratio, and mix them to form the material reaction solution A-1 ,spare;

[0025] 2) At 20°C, take 10 parts of anhydrous aluminum trichloride, 1 part of concentrated sulfuric acid, 0.5 parts of hydrochloric acid, and 2 parts of cyclohexane according to the ratio of parts by weight, and first mix the concentrated sulfuric acid, hydrochloric acid and cyclohexane , and then add anhydrous aluminum trichloride while stirring to form a reaction mixture A-2 after the reaction is terminated, for subsequent use;

[0026] 3) According to the ratio of parts by weight, take 1 part of the material reaction solution A-1 and gradually add it dropwise to 1.2 parts of the reaction mixture A-2. The dropping time is 50 minutes. After the dropping is completed, use thin-layer chromatogra...

Embodiment 2

[0036] Step 1, preparation of intermediate 1,1,3,4,4,6-hexamethyltetralin

[0037] 1) Take 2.5 moles of p-cymene, 1.25 moles of 2,3-dimethyl-1-butene and 1.25 moles of tert-butyl chloride according to the molar mass ratio, and mix them to form the material reaction solution A-1 ,spare;

[0038] 2) At 23°C, take 10 parts of anhydrous aluminum trichloride, 1 part of concentrated sulfuric acid, 0.5 parts of hydrochloric acid, and 3 parts of cyclohexane according to the ratio of parts by weight, and first mix the concentrated sulfuric acid, hydrochloric acid and cyclohexane , and then add anhydrous aluminum trichloride while stirring to form a reaction mixture A-2 after the reaction is terminated, for subsequent use;

[0039] 3) According to the ratio of parts by weight, take 1 part of the material reaction solution A-1 and gradually add it dropwise to 1.3 parts of the reaction mixture A-2. The dropping time is 60 minutes. After the dropping is completed, use thin-layer chromatog...

Embodiment 3

[0049] Step 1, preparation of intermediate 1,1,3,4,4,6-hexamethyltetralin

[0050] 1) Take 3 moles of p-cymene, 1.5 moles of 2,3-dimethyl-1-butene and 1.40 moles of tert-butyl chloride according to the molar mass ratio, and mix them to form the material reaction solution A-1 ,spare;

[0051] 2) At 25°C, take 10 parts of anhydrous aluminum trichloride, 1 part of concentrated sulfuric acid, 0.5 parts of hydrochloric acid, and 4 parts of cyclohexane according to the ratio of parts by weight, and first mix the concentrated sulfuric acid, hydrochloric acid and cyclohexane , and then add anhydrous aluminum trichloride while stirring to form a reaction mixture A-2 after the reaction is terminated, for subsequent use;

[0052] 3) According to the ratio of parts by weight, take 1 part of the material reaction solution A-1 and gradually add it dropwise to 1.5 parts of the reaction mixture A-2. The dropping time is 70 minutes. After the dropping is completed, use thin-layer chromatograp...

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Abstract

The invention relates to a preparation method of industrial musk tonalide, which comprises the following steps: carrying out Friedel-Crafts alkylation by using p-isopropyl toluene and 2,3-dimethyl-1-butene as raw materials and using tertiary butyl chloride as a hydrogen absorption agent to synthesize an intermediate 1,1,3,4,4,6-hexamethyl tetrahydronaphthalene; and in a dichloromethane solvent, carrying out Friedel-Crafts alkylation on the intermediate used as the raw material and acetyl chloride, thereby obtaining the product musk tonalide (7-acetyl-1,1,3,4,4,6-hexamethyl tetrahydronaphthalene, AHMT). Compared with the existing method and technology, the method provided by the invention is simple to operate, has the characteristics of high reaction speed, high yield and the like, and realizes industrial production; and the product can be simply purified by thermally dissolving out pigments by using anhydrous alcohol without distillation or rectification.

Description

technical field [0001] The invention relates to a synthesis method of musk, in particular to a preparation method of industrial breathing musk. Background technique [0002] Tuna musk (7-acetyl-1,1,3,4,4,6-hexamethyltetrahydronaphthalene) is a daily-use fragrance, Tuna musk belongs to the bicyclic tetralin musk, with a strong Powder scent, excellent quality, elegant aroma, long-lasting fragrance, giving people a very comfortable and pleasant feeling, the product has strong diffusivity, good coordination, stable in acid-base medium, not easy to change color, strong adhesion to fibers , suitable for high-end cosmetics such as soaps and face powders, as well as detergents and fabric softeners. This product is internationally recognized as a very ideal fragrance that is safe to use and harmless to human skin. The development and research of nitro musk is still in its infancy, and it still needs to be imported from abroad. At present, nitro musk is often used in the domestic mar...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C49/792C07C45/46
Inventor 尹卫平邓瑞雪吴秀芹刘普段文录
Owner HENAN UNIV OF SCI & TECH
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