Synthesis method of 1, 1, 3, 5-tetramethyl-3-isopropyl hydrindene

Abstract

The invention relates to a synthetic method of 1, 1, 3, 5-tetramethyl-3-isopropyl hydrindene. The synthetic method specifically comprises the following steps: S1, uniformly mixing p-cymene, chlorotert-butane and 2, 3-dimethyl-1-butene, dropwise adding an obtained mixed solution into a reaction kettle filled with cyclohexane and aluminum trichloride, stirring for reaction, washing with water and alkali for elution, and rectifying to remove p-cymene, so as to obtain a 1, 1, 3, 4, 4, 6-hexamethyltetrahydronaphthalene crude product; S2, transferring the 1, 1, 3, 4, 4, 6-hexamethyl tetrahydronaphthalene crude product obtained in the step S1 into an isomerization kettle, then adding dichloroethane and aluminum trichloride, and carrying out stirring, heating and reflux reaction; S3, washing a product obtained after the isomerization reaction with water and alkali until the product is neutral, desolventizing to remove dichloroethane, transferring an obtained desolventized 1, 1, 3, 5-tetramethyl-3-isopropyl hydrindene crude product into a crystallization kettle, adding a crystallization solvent, and recrystallizing for multiple times to obtain the 1, 1, 3, 5-tetramethyl-3-isopropyl hydrindene. According to the synthetic method of the 1, 1, 3, 5-tetramethyl-3-isopropyl hydrindene, provided by the invention, the yield of a target product is improved, and the purification difficulty is reduced.

Description

technical field

[0001] The invention relates to the technical field of synthesis of polycyclic musk intermediates, in particular to a synthesis method of 1,1,3,5-tetramethyl-3-isopropylindane. Background technique

[0002] Polycyclic musks have been widely used in the fields of cosmetics, detergents, perfumes and medicines. Because of its stable acid and alkali resistance, it has become one of the most promising synthetic musks. There is also a slight musky aroma after melting;

[0003]

[0004] Usually the synthetic technique of indane structure has: substituent benzene and olefin form indane (US4877912) under the catalysis of protonic acid or Lewis acid; The preparation method of powder sandalwood musk. According to the above direct synthesis of 1,1,3,5-tetramethyl-3-isopropylindane, firstly, the olefins and alcohols required by the raw materials are difficult to obtain, and secondly, the reaction yield is low, about 20-25%. According to the synthesis of the indane ...

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