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Modified method for preparing sclareolide from sclareol

A technology of sclareolide and sclareolide, applied in the direction of organic chemistry and the like, can solve problems such as residue and loss of sclareolide, and achieve the effects of simple operation, improved total yield, and improved commercial value

Inactive Publication Date: 2011-09-28
EAST CHINA UNIV OF SCI & TECH
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  • Abstract
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  • Claims
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Problems solved by technology

In this way, there will be a certain amount of sclareolactone remaining in the crystallization mother liquor, causing "loss"

Method used

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  • Modified method for preparing sclareolide from sclareol

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Embodiment 1

[0024] Get the crystallization mother liquor of sclareolide (provided by a certain factory, take potassium permanganate as the crystallization mother liquor of the sclareolide synthesized as a catalyst, the content of sclareolide in the crystallization mother liquor is 10wt%~30wt%) 40ml , add 80ml of methanol to get 66mg / ml methanol solution of sclareolactone, add resin HZ-84530g, perform static adsorption at normal temperature (20℃~25℃) and normal pressure (1atm) for 4 hours for pretreatment to remove some impurities . Filter out the liquid and then add resin HZ-81630g, after static adsorption at room temperature (20°C-25°C) and normal pressure (1atm) for 8 hours, use 150ml of borax-NaOH mixed solution with pH value of 9.2, 200ml Wash with deionized water, filter to obtain dry resin, the resin adsorption capacity is 247mg / dry resin g, and the adsorption rate is 92.6%. The adsorbed 30g HZ-816 resin is packed into a column, and the eluent of cyclohexane: butyl acetate: methano...

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Abstract

The invention relates to a preparation method of sclareolide, comprising the following steps of: (a). oxidizing sclareol to obtain a crude sclareolide product; and (b) crystallizing the crude sclareolide product obtained in the step (a) to obtain a pure sclareolide product. The preparation method is characterized in that sclareolide is recovered and processed from crystallization mother liquor obtained in the step (b), and the obtained sclareolide is mergered into the step (b) and crystallized and purified together with the synthesized crude sclareolide product. The invention adopts the environment-friendly method with simple operation, realizes the purpose of recovering sclareolide from the sclareolide crystallization mother liquor, improves the total recovery of the sclareolide and establishes a solid foundation for improving the commercial value of the sclareolide.

Description

technical field [0001] The invention relates to a method for preparing sclareolide, in particular to a method for preparing sclareolide from sclareol through a chemical synthesis method. Background technique [0002] Sclareolide, whose structure is shown in formula I, has been widely used in industries such as food, wine and tobacco as a spice component. Therefore, the method for large-scale preparation of high-purity sclareolide has attracted much attention. [0003] [0004] At present, the methods for preparing sclareolide are mainly divided into two categories, one is chemical synthesis methods, such as the methods disclosed in U.S. Pat. No. 5,525,728 and U.S. Pat. No. 5,247,100. The main steps of this type of method are: using a ruthenium catalyst and an oxidation step to convert sclareol into the crude product of sclareolide; the second is a biological fermentation method, such as using Cryptococcus albidus, Bensigntonia ciliata to convert sclareol (also known as ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/92
Inventor 陈葵周敏武斌纪利俊吴艳阳朱家文
Owner EAST CHINA UNIV OF SCI & TECH
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