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Preparation of isobenzofuran ketone compounds

A technology for furanones and compounds is applied in the field of preparation of isobenzofuranones, and can solve the problems of low purity and low recovery rate.

Inactive Publication Date: 2008-12-17
XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The existing preparation methods of isobenzofuranone compounds are mainly separated from microorganisms or plants by column chromatography or obtained by total synthesis, but there are problems of low recovery rate and low purity.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] a. Take 500 g of defatted Nigella seeds, then use 50% ethanol to extract by means of microwave extraction, and the extract is concentrated under reduced pressure until it has no alcohol smell, so as to obtain the total extract;

[0017] b. Disperse the total extract in water, extract sequentially with petroleum ether, chloroform, ethyl acetate, and n-butanol, and arrange under reduced pressure to obtain petroleum ether, chloroform, ethyl acetate, and n-butanol respectively, and then take The ethyl acetate part is the raw material for subsequent use;

[0018] c. Prepare a solvent system formed by four components, put petroleum ether, ethyl acetate, acetonitrile and water in a separatory funnel in a volume ratio of 3:4:5.5:4, shake well and let stand to separate layers. After equilibration, separate the upper and lower phases for later use;

[0019] d. Weigh 200 mg of the ethyl acetate part of the raw material in step b, dissolve it in the solvent system prepared in step...

Embodiment 2

[0021] a. Take 400 g of defatted Nigella seeds, then use 70% ethanol to extract by ultrasonic extraction at room temperature at a temperature of 20° C., extract the extract under reduced pressure until it has no alcohol smell, and obtain the total extract;

[0022] b. Disperse the total extract in water, extract sequentially with petroleum ether, chloroform, ethyl acetate and n-butanol, and arrange under reduced pressure to obtain the petroleum ether part, chloroform part, ethyl acetate part and n-butanol part respectively, and then take chloroform parts are raw materials;

[0023] c. prepare a solvent system formed by four components, put n-pentane, ethyl acetate, methanol and water in a volume ratio of 5:5:4.5:5 in a separatory funnel, shake it up and let it stand for stratification. After equilibration, separate the upper and lower phases;

[0024] d. Weigh 600 mg of the chloroform part of the raw material in step b, dissolve it in the solvent system prepared in step c for...

Embodiment 3

[0026] a. Take 500 g of defatted Nigella seeds, then use 60% ethanol to extract at room temperature by means of normal temperature leaching, the extract is concentrated under reduced pressure until it has no alcohol smell, and the total extract is obtained;

[0027] b. Disperse the total extract in water, extract sequentially with petroleum ether, chloroform, ethyl acetate and n-butanol, and arrange under reduced pressure to obtain the petroleum ether part, chloroform part, ethyl acetate part and n-butanol part respectively, and then take acetic acid The ethyl ester part is the raw material;

[0028] c. Prepare a solvent system formed by four components, put n-hexane, ethyl acetate, ethanol and water in a separatory funnel in a volume ratio of 6:2.5:3:4, shake well, let stand to separate layers, and wait for equilibrium After that, separate the upper and lower phases;

[0029] d. Weigh 200 mg of ethyl acetate, the raw material of step b, and dissolve it in the solvent system ...

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Abstract

The invention relates to a preparation method for obtaining isobenzofuran ketone compound from a crude extract of a fennelflower by adopting a method of high-speed countercurrent chromatography. A solvent used by the preparation method of the invention is petroleum ether or n-hexane or n-heptane or a four-component solvent system composed of n-pentane, acetic ether and methanol or ethanol or methyl cyanide and water and the isobenzofuran ketone compound is separated from the fennelflower by a separation step. The method has lager separation amount, no damage to samples, high recovery rate and moderate separation environment, and saves the solvent. Adoption of a countercurrent chromatograph can ensure that a large amount of crude samples can be brought in directly or compounded to a compound and the separation can realize higher purity and obtain good separation effect. The preparation method of the invention is not only applicable to preparing products with higher purity from the crude extract of plants but also applicable to purifying the crude extract of isobenzofuran ketone substances which are obtained through various means and separating the isobenzofuran ketone substances by the countercurrent chromatographs of different types.

Description

technical field [0001] The invention relates to a preparation method for separating isobenzofuranone compounds from black cumin crude extract by high-speed countercurrent chromatography. Background technique [0002] Nigella is a plant of the Ranunculaceae Nigella genus, which is a commonly used medicinal material in Uighur medicine. It has the effects of stimulating digestion, dispelling wind and relieving pain, tonifying kidney and brain, diuresis, sweating, invigorating stomach, anti-worm, treating asthma, stimulating menstruation, and promoting milk. [0003] Since 1959, there have been more than 200 studies on Nigella. Foreign studies have confirmed that Nigella nigella has anti-infection, rheumatism, analgesic, estrogen-like activity, anti-ulcer, anti-virus, anti-bacterial, fungal, lipid-lowering and hypoglycemic effects, and can treat kidney stones and enhance immunity , enhance heart function, treat asthma, etc. Studies in recent years have shown that in addition ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/88
Inventor 阿吉艾克拜尔·艾萨信学雷杨义
Owner XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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