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Preparation method of 5,15-O-diacetyl-3-O-nicotinoyl-lathyrol

A technology of diacetyl and caperin alcohol, which is applied in the direction of organic chemistry, can solve the problems of hindering 3-O-nicotinoyl, which is difficult to realize, and achieve the effect of high separation efficiency, high operability and stable process

Inactive Publication Date: 2015-03-25
TIANJIN YAOYU BIOLOGICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] But so far, there is no report on the method of extracting 3-O-nicotinoyl-5,15-O-diacetyl capserol in natural product extracts by liquid chromatography. The body 3-O-nicotinoyl-5,15-O-diacetyl capserol is more difficult to achieve, which also hinders the 3-O-nicotinoyl-5,15-O-diacetyl Progress in the development of Caperol as a traditional Chinese medicine

Method used

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  • Preparation method of 5,15-O-diacetyl-3-O-nicotinoyl-lathyrol

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Embodiment 1

[0033] 1. Obtaining the primary extract of QJZ

[0034] 1. Crushing:

[0035] Take Qianjinzi as a raw material, put it into a pulverizer for pulverization.

[0036] 2. Organic reagent extraction:

[0037] The stephenia powder was extracted with organic reagents, three consecutive extractions, each extraction time was 6h (heated to 60 degrees, and then heated for 6h). specific:

[0038] The first organic reagent extraction: add 2.5 kg of Stephania chinensis powder to 20 L of organic reagent, the organic reagent is ethyl acetate, stir well until the material liquid is uniform and there are no obvious lumps, turn on the water bath, extract for 6 hours, after the extraction is completed, collect the The supernatant was filtered with filter paper, and the supernatant was concentrated in a rotary evaporator and then transferred to a constant temperature blast drying oven at 60°C for drying to obtain the initial QJZ extract, which was precipitated for use;

[0039] The second org...

Embodiment 2

[0046] 1. Obtaining the primary extract of QJZ

[0047] 1. Crushing:

[0048] Take Qianjinzi as a raw material, put it into a pulverizer for pulverization.

[0049] 2. Organic reagent extraction:

[0050] The stephenia powder was extracted with organic reagents, three consecutive extractions, each extraction time was 6h (heated to 60 degrees, and then heated for 6h). specific:

[0051] The first organic reagent extraction: add 2.5 kg of Stephania chinensis powder to 20 L of organic reagent, the organic reagent is ethyl acetate, stir well until the material liquid is uniform and there are no obvious lumps, turn on the water bath, extract for 6 hours, after the extraction is completed, collect the The supernatant was filtered with filter paper, and the supernatant was concentrated in a rotary evaporator and then transferred to a constant temperature blast drying oven at 60°C for drying to obtain the initial QJZ extract, which was precipitated for use;

[0052] The second org...

Embodiment 3

[0059] 1. Obtaining the primary extract of QJZ

[0060] 1. Crushing:

[0061] Take Qianjinzi as a raw material, put it into a pulverizer for pulverization.

[0062] 2. Organic reagent extraction:

[0063] The stephenia powder was extracted with organic reagents, three consecutive extractions, each extraction time was 6h (heated to 60 degrees, and then heated for 6h). specific:

[0064] The first organic reagent extraction: add 2.5 kg of Stephania chinensis powder to 20 L of organic reagent, the organic reagent is ethyl acetate, stir well until the material liquid is uniform and there are no obvious lumps, turn on the water bath, extract for 6 hours, after the extraction is completed, collect the The supernatant was filtered with filter paper, and the supernatant was concentrated in a rotary evaporator and then transferred to a constant temperature blast drying oven at 60°C for drying to obtain the initial QJZ extract, which was precipitated for use;

[0065] The second org...

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Abstract

The invention relates to a preparation method of 5,15-O-diacetyl-3-O-nicotinoyl-lathyrol. According to the preparation method, 5,15-O-diacetyl-3-O-nicotinoyl-lathyrol is extracted from seeds of euphorbia lathyris with a two-dimensional liquid-phase chromatographic technique, by means of complementary separation which is realized through reasonable selection of chromatographic columns, dissolved solutions, mobile phases and the like, optimization of technological conditions such as the flow velocity, the elution mode, the collection sections and the like as well as orthogonality of the first dimension and the second dimension, the whole separation and purification method is practicable, the operability is high, the purity of the obtained 5,15-O-diacetyl-3-O-nicotinoyl-lathyrol is high and can be higher than 96% at most, the technology of the whole process is stable, the operation is simple and convenient, and the separation efficiency is high.

Description

technical field [0001] The invention relates to the field of compound production, in particular to a preparation method of 3-O-nicotinoyl-5,15-O-diacetyl caperin alcohol. Background technique [0002] Qianjinzi is the dried and mature seed of Euphorbia lathyris, a plant of the Euphorbia family, which is one of the traditional Chinese medicinal materials in my country. Fructus Qianjinzi is warm in nature, pungent in taste, and slightly poisonous. Its main functions are to expel water to reduce swelling and eliminate blood stasis. , warts. In foreign countries, the plant seeds have long been used for cancer treatment records, and its methanol extract has been shown to have anti-cancer effects in preliminary screening assays for anti-malignant tumor-related activities. 3-O-nicotinoyl-5,15-O-diacetyl-caprolol is one such compound, which is an important natural active ingredient widely present in Euphorbiaceae plants, and its structure is as follows: [0003] [0004] More ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/80C07D213/803
CPCC07D213/80C07D213/803
Inventor 张耀洲杨珊珊顾朋嫒李聪聪
Owner TIANJIN YAOYU BIOLOGICAL TECH
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