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Synthetic method of perfume o-tert-butylcyclohexyl acetate

A technology of tert-butyl cyclohexyl ester and tert-butyl cyclohexanol, applied in the field of chemical synthesis, can solve the problems of unsuitability for large-scale production, severe reaction conditions, low reaction yield and the like, and achieves fine product aroma, high reaction yield and easy operation. Safe and convenient effect

Inactive Publication Date: 2013-07-10
南昌洋浦天然香料香精有限公司
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AI Technical Summary

Problems solved by technology

[0003] O-tert-butylcyclohexyl acetate is often used in soap essence and cosmetic essence formulations because of its floral and fruity aroma. The traditional production method of o-tert-butylcyclohexyl acetate has severe reaction conditions, inconvenient operation and low reaction yield. , not suitable for industrial mass production

Method used

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Embodiment Construction

[0011] This specific embodiment takes the following technical solutions: 1. Synthesis of o-tert-butylphenol: in a three-necked flask equipped with a thermometer, an electric stirrer, a gas conduit, and a drying tube, add 113g of phenol, concentrated H 2 SO 4 2.3g, anhydrous AlCl 3 9g, heat up to 50°C, under strong stirring, feed isobutene gas, stop feeding isobutene when the weight of the reactant reaches about 62g, then raise the temperature to 80°C, stir and react for 2 hrs, wash with 230ml×2 hot water The reactant was evaporated to remove water under reduced pressure with a water jet pump, and then the crude product was steamed out by vacuum distillation, and the resulting crude product was recrystallized with 240ml of petroleum ether, frozen, filtered, and dried to obtain 128g of o-tert-butylphenol;

[0012] 2. Synthesis of o-tert-butylcyclohexanol: put a three-neck flask equipped with a thermometer, an electric stirrer, a dropping funnel and a gas conduit on a water ba...

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Abstract

The invention relates to a chemical synthetic method, and concretely relates to a synthetic method of a perfume o-tert-butylcyclohexyl acetate. The synthetic method comprises the following steps: reacting a raw material phenol with isobutene under the catalysis of anhydrous aluminum trichloride to obtain o-tert-butyl phenol, carrying out catalytic hydrogenation of o-tert-butyl phenol under the catalysis of Raney nickel to obtain o-tert-butyl cyclohexanol, and carrying out an esterification reaction of o-tert-butyl cyclohexanol and acetic anhydride under the catalysis of anhydrous sodium acetate to obtain o-tert-butylcyclohexyl acetate. The method has the advantages of mild reaction conditions, safe and convenient operation, high reaction yield, fine and strong fragrance of the obtained product, raw material source enlargement and raw material cost saving because of the adoption of industrially cheap phenol and isobutene as initial raw materials, total synthetic reaction yield improvement, suitableness for the industrial adoption, and good economic benefit.

Description

technical field [0001] The invention relates to a chemical synthesis method, in particular to a spice o-tert-acetic acid [0002] The synthetic method of butyl cyclohexyl ester. Background technique [0003] O-tert-butylcyclohexyl acetate is often used in soap essence and cosmetic essence formulations because of its floral and fruity aroma. The traditional production method of o-tert-butylcyclohexyl acetate has severe reaction conditions, inconvenient operation and low reaction yield. , not suitable for large-scale industrial production. [0004] Contents of the invention [0005] The purpose of this invention is to provide a kind of synthetic method of perfume o-tert-butylcyclohexyl acetate, which has mild reaction conditions, safe and convenient operation, high reaction yield, and more delicate and strong product aroma; it adopts industrially cheap and easy-to-obtain phenol and Isobutene is used as the starting raw material, which expands the source of raw materials,...

Claims

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Application Information

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IPC IPC(8): C07C69/14C07C67/08
Inventor 梅家庆
Owner 南昌洋浦天然香料香精有限公司
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