Preparation method of template agent intermediate 4,5-dimethyl bicyclo[2.2.2] octane-2-alcohol

Abstract

The invention relates to a preparation method of 4,5-dimethyl bicyclo[2.2.2] octane-2-alcohol. The preparation method of the 4,5-dimethyl bicyclo[2.2.2] octane-2-alcohol comprises the following steps: 1) carrying out reaction on 3-methyl-2-cyclohexene-1-ketone and a lithium reagent, then carrying out reaction with trimethylchlorosilane, so that trimethyl (5-methyl cyclohexene-1-5-dialkylene oxyl) silane is generated; 2) carrying out Diers-Alder reaction on trimethyl (5-methyl cyclohexene-1-5-dialkylene oxyl) silane and acrylonitrile, and hydrolyzing for generating 1-methyl-5-ketone bicycle[2.2.2]octane-2-cyanogen; 3) carrying out reaction on 1-methyl-5-ketone bicycle[2.2.2]octane-2-cyanogen and hydrogen under the catalytic action of palladium on carbon, so that the 4,5-dimethyl bicyclo[2.2.2] octane-2-alcohol is obtained. The preparation method of the 4,5-dimethyl bicyclo[2.2.2] octane-2-alcohol has the advantages that a three-step reaction process is adopted, the total yield of each reaction step is more than 85%, purity is respectively more than 88%, purity of a product of a middle step can be 97.3, and steps are simple; meanwhile, lithium aluminium hydride is not used in the reaction process, and aftertreatment is simple, so that the preparation method of the 4,5-dimethyl bicyclo[2.2.2] octane-2-alcohol is more applicable to industrial production; purification through column chromatography does not need to be carried out, time and labour are saved, purity is high, and cost is saved.

Description

Technical field [0001] The invention relates to a preparation method of a template intermediate 4,5-dimethylbicyclo[2.2.2]octan-2-ol, which belongs to the field of molecular sieves. Background technique [0002] Zeolite molecular sieve materials, especially silica alumina zeolite molecular sieve materials, have regular microporous channels, large specific surface area, high thermal stability and hydrothermal stability, and are currently the most widely used heterogeneous catalytic materials in the petrochemical industry . In the synthesis of modern zeolite molecular sieves, the use of organic template agents plays a very important role. The development of new topology zeolite molecular sieves and the exploration of new synthetic routes are closely related to new template molecules. Usually, template molecules are used in the synthesis of zeolite molecular sieves. Plays the role of structure guidance, pore filling and balance of skeleton charge. [0003] In recent years, the SSZ-1...

AI Technical Summary

Problems solved by technology

The dangerous flammable lithium aluminum tetrahydrogen (LiAlH 4 ) as a reducing agent greatly reduces the safety of the entire synthetic route, and is not suitable for workshop production amplification; and when p-toluenesulfonyl chloride is esterified, it needs to be purified by column chromatography, which not only wastes man-hours, but also reduces the yield. make the product cost higher

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