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Method for preparing aromadendrane-4 beta, 10 alpha-diol

A technology of soft corals and pods, applied in the field of medicine, can solve problems such as the difficulty of industrial production, and achieve the effect of broad application prospects

Inactive Publication Date: 2018-10-19
龚小青
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Problems solved by technology

However, the current methods for preparing Alismoxide, ent-spathulenol, 4α, 10α-aromadendranediol, and aromadendrane-4β, 10α-diol all rely on silica gel column chromatography and / or gel column chromatography, a separation medium that cannot be applied industrially. Difficult to produce

Method used

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  • Method for preparing aromadendrane-4 beta, 10 alpha-diol
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  • Method for preparing aromadendrane-4 beta, 10 alpha-diol

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Embodiment Construction

[0031] The content of the present invention will be described in detail below in conjunction with the accompanying drawings and embodiments.

[0032] The pod soft coral (Lobophytum sp.) was collected at 20m underwater in the waters of West Island, Sanya, Hainan, my country, and was immediately frozen for later use.

[0033] TBE-300 high-speed countercurrent chromatography was purchased from Shanghai Tongtian Biochemical Technology Co., Ltd.

[0034] The method for preparing Alismoxide, ent-spathulenol, 4α, 10α-aromadendranediol, aromadendrane-4β, 10α-diol comprises the following steps:

[0035] Step S1, extraction and concentration:

[0036] First cut up the soft coral pods, freeze-dry, and then extract the dried soft coral pods by cold soaking with petroleum ether for 3 times (solid-to-liquid ratio: 1:30), each time for 8 hours, collect the soft coral pods, and then heat reflux with acetone Extract 3 times (solid-to-liquid ratio is 1:20), each time 2h, collect acetone extra...

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Abstract

The invention discloses a method for preparing aromadendrane-4 beta, 10 alpha-diol. The method comprises the steps of: step S1, extracting and concentrating to obtain a pod alcyonacea acetone extract;step S2, enriching the acetone extract with XDA-1B macroporous resin, firstly eluting with 30% ethanol, then eluting with 65% ethanol, collecting 4.5 to 5.0 BV of 65% ethanol eluate, and concentrating and drying to obtain an enriched material; step S3, taking ethyl acetate-normal butanol-trifluoroacetic acid-water as a solvent system for high-speed countercurrent separation of the enriched material. The method does not rely on silica gel column chromatography and / or gel column chromatography, and has broad application prospects.

Description

technical field [0001] The invention belongs to the field of medicine, and in particular relates to a preparation method of several medicinally active compounds. Background technique [0002] The chemical formulas of Alismoxide, ent-spathulenol, 4α,10α-aromadendranediol, and aromadendrane-4β,10α-diol are shown below. Alismoxide was first disclosed by literature (Terpenoids of Alisma orientalerhizome and the crude drug Alismatis rhizoma. Phytochemistry, 1994). ent-spathulenol was first disclosed by literature (Three ent-secoaromadendrane-type sesquiterpenehemiacetals and a bicyclogermacrene from Plagiochilaovalifolia and Plagiochilayokogurensis. Phytochemistry, 1980). 4α, 10α-aromadendranediol and aromadendrane-4β, 10α-diol were first published in the literature (Sesquiterpene lactonesanda sesquiterpene diol from jamaican ambrosia peruviana. Phytochemistry, 1987). [0003] [0004] Studies have found that Alismoxide, ent-spathulenol, 4α, 10α-aromadendranediol, and aromad...

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Application Information

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IPC IPC(8): C07C29/76C07C35/34C07C35/37
CPCC07C29/76C07C2602/30C07C2603/30C07C35/34C07C35/37
Inventor 龚小青
Owner 龚小青
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