Method of synthesizing tricyclodecenyl isobutyrate spice

Abstract

A method of synthesizing tricyclodecenyl isobutyrate spice relates to the technical filed of fine chemical engineering synthesis. In the invention, with dicyclopentadiene and isobutyric acid in approximate equimolar proportion as raw materials, with zeolite-carrying phosphotungstic acid as a catalyst and with isobutyric anhydride as a protective agent, the tricyclodecenyl isobutyrate is synthesized. An acetylation reaction is directly carried out to prepare a crude product of the tricyclodecenyl isobutyrate by one step through electrophilic addition under catalysis of a catalyst. Meanwhile, a less amount of the isobutyric anhydride is added for protecting the catalyst, and then the isobutyric acid is recycled and reused so that a finish product of the tricyclodecenyl isobutyrate is obtained through neutralization washing and rectification. The method can solve problems that the spice has a sour smell in fragrance and the quality of the spice is influenced since a method in the prior art pollutes environment, is complex in post-treatment process, causes equipment corrosion and is uncooperative in ratio of isomers. The method employs the raw materials being easy to get, is mild in conditions, is high in conversion rate, is convenient to carry out, is high in yield, is less in emission of waste gas, waste water and solid waste during production and belongs to a clean production process.

Description

technical field [0001] The invention relates to the technical field of fine chemical synthesis, in particular to a method for synthesizing tricyclodecenyl isobutyrate perfume. Background technique [0002] The appearance of tricyclodecenyl isobutyrate is a colorless to light yellow liquid. Tricyclodecenyl isobutyrate is a mixture of four isomers, and its main components include tricyclic [5,2,1,0 2.6 ]-8-Decen-3-ol isobutyrate, Tricyclo[5,2,1,0 2.6 ]-3-Decen-9-ol isobutyrate, Tricyclo[5,2,1,0 2.6 ]-3-Decen-8-ol isobutyrate, Tricyclo[5,2,1,0 2.6 There are four isomers of ]-8-decen-4-ol isobutyrate. Due to the different positions of the acetoxy groups, the top aroma of the product is either fruity or herbal. The flash point is 110℃, the relative density is 1.024~1.028(25 / 25℃), and the refractive index is 1.482~1.487(20℃). Tricyclodecenyl isobutyrate has a sweet fruity and herbal aroma in daily chemical flavors, and is an important synthetic fragrance in the cycloalkene fam...

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Problems solved by technology

[0010] The present invention proposes a synthesis method of tricyclodecenyl isobutyrate perfume, the purpose of which is to solve the environmental pollution existing in the prior art, the use of a large amount of excess isobutyric acid leads to complicated post-treatment process, equipment corrosion and the ratio of isomers Uncoordinated, resulting in the problem that the aroma has a sour taste and affects the quality of the product. The raw materials are easy to obtain, the reaction conditions are mild, the reaction conversion rate is high, the process is easy to implement, the product yield is high, and the three wastes in the production process are less discharged and efficient. Environmentally friendly, at the same time, the product has a fruity and sweet tricyclic [5,2,1,0 2.6 The content of ]-3-decen-9-ol isobutyrate reaches more than 92%. The aroma of the product is pure, delicate and soft, and the product quality and aroma quality can meet the market demand.

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