Preparation method of tonalide intermediate HMT

Abstract

The invention provides a preparation method of a tonalide intermediate HMT. The preparation method comprises the steps of mixing p-cymene, sulfuric acid, phosphoric acid and aluminum trichloride in acertain ratio in a reactor; then mixing and dripping 2,3-dimethyl-1-butene and tert-butyl chloride into the reactor, and reacting at a room temperature for 1 hour to generate the tonalide intermediateHMT, wherein the molar ratio of 2,3-dimethyl-1-butene to tert-butyl chloride to p-cymene to aluminum trichloride to sulfuric acid to phosphoric acid to dichloroethane to cyclohexane is 0.5-1.5 to 0.9-1.3) to 1.4-2.6 to 0.07-0.13 to 0.006-0.013 to 0.006-0.012 to 0.7-1.5 to 0.6-1.4; and directly transferring the reacted substances to a rectification column for rectification and purification to obtain a tonalide intermediate HMT product. The HMT product with higher yield can be obtained from new reaction substances, the purification method is improved, and the conventional recrystallization purification method is changed to reduce pollution and lower the production cost.

Description

technical field [0001] The present invention relates to the field of preparation of HMT, an intermediate of Tuna musk, and more specifically, relates to a preparation method of HMT of Tuna musk intermediate. Background technique [0002] Tonalide is a synthetic musk with tetralin structure. It has excellent fragrance quality, elegant fragrance, long-lasting fragrance, acid and alkali resistance, no discoloration under natural light, strong diffusion power, and no stimulation to human skin. It has good compatibility with other fragrances and is an ideal fragrance raw material. It is widely used in the fields of cosmetics, perfume, tobacco, essence and medicine, and has become one of the most promising synthetic musk products; [0003] The chemical name of Tuna musk is 7-acetyl-1,1,3,4,4,6-hexamethyl-1,2,3,4-tetrahydronaphthalene (abbreviated as AHMT), usually composed of intermediate 1, 1,3,4,4,6-hexamethyltetrahydronaphthalene (referred to as HMT) and acetylation reagents s...

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Problems solved by technology

[0003] The chemical name of Tuna musk is 7-acetyl-1,1,3,4,4,6-hexamethyl-1,2,3,4-tetrahydronaphthalene (abbreviated as AHMT), usually composed of intermediate 1, 1,3,4,4,6-hexamethyltetrahydronaphthalene (referred to as HMT) and acetylation reagents such as acetyl chloride or acetic anhydride are prepared by Friedel-Crafts reaction under Lewis acid catalysis; among them, HMT is very important Reactants, so the demand for HMT is very high, most of the existing HMT is prepared in two ways, one is: using raw materials 2,3-dimethyl-1-butene and tert-butyl chloride, p-cymene Reaction in catalyst aluminum chloride, solvent dichloromethane reaction at low temperature for about 4 hours to get product HMT, reaction yield 40%-50%; the second is: use raw material 3,3-dimethyl-1-butene Tert-butyl chloride reacts with cymene in the reaction of catalyst aluminum trichloride and solvent dichloromethane for about 4 hours to obtain the product HMT, and the reaction yield is 60%-70%; although the above two preparation methods can obtain HMT , but the reaction yields are not ideal, and some materials are difficult to obtain, and the cost is high; and in the prior art, most of the purification of HMT adopts the method of recrystallization, which needs to consume corresponding solvents, and the production of substances is likely to cause environmental pollution

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