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Method for preparing epoxy myrcene

A technology of epoxy myrcene and myrcene, which is applied in the field of preparation of epoxy myrcene, can solve problems such as difficult separation and purification of products, and achieve the effects of safe operation, low cost and excellent product performance

Inactive Publication Date: 2007-07-25
上海力智生化科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

If the above method is used to epoxidize such a raw material to prepare epoxymyrcene, it will definitely bring many difficulties to the separation and purification of the product.

Method used

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  • Method for preparing epoxy myrcene
  • Method for preparing epoxy myrcene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Preparation of myrcene sulfone: add 200g myrcene (industrial product, content about 75%, 1.1mol), 2g (9mmol) 2,6-di-tert-butyl-4-methylphenol and 200g (3.1mol) in the autoclave Sulphur dioxide. Heating and stirring, the temperature is controlled at 65 ~ 75 ℃. After the pressure in the reactor was stable and no longer decreased, the reaction was continued for 2 hours. After the reaction is completed, the remaining sulfur dioxide in the reactor is vented, and the vented gas is absorbed by alkaline water.

[0028] The obtained reactant was subjected to vacuum distillation, and the fractions before 85°C / 5mmHg were impurities that did not participate in the reaction in the raw materials, and they were removed as much as possible. The residue is the crude product of myrcyl sulfone with a purity of about 90-95%. According to the actual content of myrcene in the raw material, the yield is close to 95%. The crude product was used in the next epoxidation reaction without furt...

Embodiment 2

[0033] Add 100g (0.5mol) myrcyl sulfone prepared in Example 1, 500mL xylene and 120g sodium percarbonate into the three-necked flask, slowly add 100mL acetic anhydride under vigorous stirring, the reaction exotherm is obvious, control the dropping rate of acetic anhydride , the reaction temperature was maintained at 40-60 °C. After the addition, the reaction was carried out at room temperature overnight, and the inorganic solid was removed. The filtrate is removed by conventional methods to remove residual peroxy compounds, and the solvent is recovered under reduced pressure to obtain a crude product of myrcene sulfone epoxidation product. The crude product was decomposed while heating, and distilled under reduced pressure, and the fractions at 75-80°C / 10mmHg were collected until the decomposition was complete. 56 g of colorless liquid were obtained in 78% yield.

[0034] Within the scope of the various components and conditions described in the method of the present inventi...

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Abstract

This invention discloses a method for preparing epoxymyrcene. The method comprises: utilizing industrial myrcene as the raw material, reacting with SO2 to form myrcenesulfone, and epoxidizing with sodium percarbonate / acetic anhydride system to obtain epoxymyrcene. The method has such advantages as stable reactions, mild conditions, safe operation, and high product quality.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and relates to a preparation method of epoxy myrcene. Background technique [0002] Epoxy myrcene (myrcene epoxide) has the fragrance of laurel, is a kind of fragrance in fine chemical industry, and is also a kind of deodorant. It is used in the flavor and fragrance industry for its pleasant laurel aroma and low aroma threshold properties. Moreover, it is also a useful intermediate, which can be converted into a series of useful derivatives by reaction (Synth. Commun., 1999, 29, 3673, Tetrahedron, 2001, 57, 1235). [0003] Epoxymyrcene is obtained by epoxidation of myrcene. The myrcene molecule contains multiple double bonds, and various epoxidation products may appear during epoxidation. But as long as the reaction conditions are properly controlled, a single 6,7-position epoxy compound can be obtained. [0004] [0005] Organic peracids are a class of effective epoxidation reag...

Claims

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Application Information

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IPC IPC(8): C07D301/02C07D303/04
Inventor 文佳赵志林陆慧
Owner 上海力智生化科技有限公司
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