1222-05-5Relevant academic research and scientific papers
Preparation method of galaxolide
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Paragraph 0010; 0037-0059, (2021/08/11)
The invention discloses a preparation method of galaxolide, which comprises the following steps: under the action of a supported cerium catalyst, carrying out alkylation reaction on 1, 1, 2, 3, 3, 5-hexamethylindane and epoxypropane, then carrying out dehydration condensation cyclization to generate galaxolide, and carrying out continuous rectification to separate the product. The problems of complex process, low raw material utilization rate, low safety and the like in the prior art are solved, the process is simple, the raw material conversion rate is greater than 95%, and the product selectivity is greater than 92%.
Preparation method of galaxolide
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Paragraph 0052-0064, (2021/02/06)
The invention discloses a preparation method of galaxolide, which comprises the following steps: carrying out methylene etherification reaction on hexamethyl indanol and a TEBBE reagent (CAS: 67719-69-1) under the action of a supported Pd catalyst, carrying out condensation cyclization to generate galaxolide, and carrying out continuous rectification to separate the product. The supported Pd catalyst is represented as Pd-X/Y, X is selected from triphenylphosphine, tributylphosphine, tricyclohexylphosphine, bis(diphenylphosphine) methane, 1, 2-bis(diphenylphosphine) ethane and 4, 5-bis(diphenylphosphin)-9,9-dimethyl xanthene, and Y is selected from carbon nanotubes, ordered mesoporous carbon, neutral alumina, silica, a molecular sieve and kaolin. The process provided by the invention avoidsthe problems of complex process, serious equipment corrosion, low safety, environmental friendliness and the like in the prior art, and the raw material conversion rate and the product selectivity can reach 93% or above.
Micro-continuous flow technology for producing tonalide
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Paragraph 0023-0036, (2020/04/17)
The invention discloses a micro-continuous flow technology for producing tonalide. The technology taking 1,1,3,4,4,6-hexamethyltetrahydronaphthalene (HMT) and acetyl chloride as raw materials, anhydrous aluminum chloride as a catalyst and dichloroethane and other organic matters as a solvent comprises the following steps: mixing the anhydrous aluminum chloride, the solvent and acetyl chloride under a low-temperature condition to obtain a catalyst phase; mixing and dissolving the raw material HMT with the solvent to obtain a raw material phase; respectively pre-cooling the raw material phase and the catalyst phase, and introducing the pre-cooled raw material phase and catalyst phase into a micro-channel reactor, and performing a reaction; and finally, introducing the obtained reaction product into a microstructure mixing module, quenching and layering the obtained reaction product, and then carrying out extraction, rotary evaporation, recrystallization and drying to obtain the tonalide.The micro-continuous flow technology has the advantages of short retention time, continuousness in operation, increase of the production efficiency of the product, improvement of the production safety and the product yield by timely removing heat in the reaction process, and reduction of the risk of the quenching process by timely removing heat in the quenching process.
Method for preparing galaxolide under catalysis of superfine aluminum trichloride
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Paragraph 0016-0017; 0019, (2019/12/25)
The invention relates to a method for preparing galaxolide under catalysis of superfine aluminum trichloride. The method is characterized by comprising the following steps: 1, adding pentamethyl indanand anhydrous aluminum trichloride with particle size of 5 meshes or blow to a solvent, and cooling the solution to subzero 30-subzero 20 DEG C, wherein the mass ratio of the pentamethyl indan to anhydrous aluminum trichloride is (1.5-2):1; 2, dropwise adding propylene oxide to dissolve in the solution in the solvent during stirring, and conducting a reaction at subzero 30-subzero 5 DEG C for 1-2h to produce hexamethyl indanol, wherein the mass ratio of the propylene oxide to pentamethyl indan is (0.3-0.5):1; 3, continuously adding a deactivating agent and formaldehyde or formaldehyde equivalents, heating the mixture to 5-65 DEG C to react for 0.5-4 h to produce galaxolide, wherein the molar ratio of the deactivating agent, the formaldehyde or formaldehyde equivalents to the pentamethylindan is (1-2):1 and (0.5-1):1; and 4, performing purification. The method has the advantages as follows: aluminum trichloride powder with superfine particle size is used, the raw material conversionrate and product yield are significantly increased, the reaction time is shortened, the reaction has good reproducibility, energy is saved, production efficiency is improved, and the production cost is reduced.
Synthetic process of galaxolide
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Paragraph 0037; 0040-0041; 0042; 0045-0046; 0050-0051, (2018/07/30)
The invention relates to a synthetic process of galaxolide. When an intermediate 1,1,2,3,3-pentamethylindane is prepared, macroporous strong-acidic styrenes cation exchanging resin prepared by the process is selected as a catalyst to react under a condition of no solvent, so that the pollution of waste gas, waste solids and waste water can be reduced, the solid catalysis is easy to separate, the industrialized production is facilitated, and the yield reaches up to 70 percent or more.
PERFUME COMPOSITIONS
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, (2011/08/06)
Perfume ingredients have been investigated and classified for their effectiveness in detaching biofilms from surfaces. Based on this classification, perfume compositions that are effective in assisting biofilm detachment can be formulated, whilst also allowing a degree of freedom in formulation that permits consideration of the hedonic properties of the composition. The compositions can be used in a wide range of perfumed consumer products, such as personal, domestic and industrial products, e.g. hard surface cleaning products, dental care products, and deodorant products.
Process for preparing isochroman compounds
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, (2008/06/13)
High-purity isochroman compounds can be obtained in high yields according to a simple and economical process for preparing isochroman compounds, comprising the step of adding an aquesous solution of formaldehyde having a concentration of 40 to 70 wt. % to a complex of an arylalkanol represented by the following general formula (II) with a Friedel-Crafts catalyst to cyclize the arylalkanol: STR1 wherein R1 and R2 each stands for a hydrogen atom, a lower alkyl group or a lower alkoxyl group, or alternatively R1 and R2 are respectively bonded to adjacent carbon atoms with mutual bonding of R1 and R2 together with the carbon atoms respectively bonded to R1 and R2 to form a benzene ring, a naphthalene ring, or a C5 or C6 cycloalkane or cycloalkene which may have 1 to 6 lower alkyl groups; and R3 stands for a hydrogen atom or a lower alkyl group.
Preparation of isochromane derivatives
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, (2008/06/13)
A process for the preparation of an isochromane of the formula STR1 in which R 1 and R 2 are identical or different and denote hydrogen, lower alkyl or lower alkoxy, or together form a cyclopentane or cyclohexane ring which is optionally substituted by lower alkyl andR 3 denotes hydrogen or lower alkyl,comprising reacting an alcohol of the formula STR2 with formaldehyde and a carboxylic acid anhydride of the formula STR3 or with a methylene diester of the formula STR4 in which R 4 represents a lower alkyl radical, in the presence of an acid catalyst. The products are known, having a musk-like odor.
