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A kind of preparation method of 6,7-epoxy ligustilide

The technology of ligustilide and epoxy is applied in the field of preparation of chemical components of traditional Chinese medicine, can solve the problems of expensive raw materials, cumbersome steps, difficult to prepare in large quantities, etc. Effect

Active Publication Date: 2020-07-10
SICHUAN ACAD OF CHINESE MEDICINE SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above method has cumbersome steps, time-consuming and labor-intensive steps, expensive raw materials, limitations in reactor volume, reaction solution concentration, etc., making it difficult to prepare a large amount of 6,7-epoxy ligustilide
This limits further research on 6,7-epoxyligustilide

Method used

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  • A kind of preparation method of 6,7-epoxy ligustilide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A kind of preparation method of 6,7-epoxy ligustilide, its steps are:

[0027] (1) Reaction: Add 100ml of water-ethanol (25:75, v / v) and 5g of volatile oil of Ligusticum chuanxiong (Ligustilide content 19.5%, w / w) into a 250ml round bottom flask in sequence, and stir at room temperature for 5 minutes. Take 10g of potassium hydrogen persulfate compound salt, slowly add it to the reaction system, stir at room temperature for 5 minutes, then place it in a water bath at 80°C for reaction, and stop the reaction when the chromatographic peak area of ​​ligustilide in the reaction solution is detected to decrease by 75%. ;

[0028] (2) Detection: Waters Acquity UPLC chromatograph; chromatographic column Waters BEH C18 (50mm×2.1mm, 1.7μm); mobile phase acetonitrile (A)–0.1% phosphoric acid water (B); gradient elution 0~0.5min (20 % A), 0.5~3.0min (20% A~70% A), 3.0-3.5min (70% A~100% A), 3.5~4.0min (100% A), 4.0~4.01min (100% A ~20% A), 4.01~5.0min (20% A); flow rate 0.4ml / min...

Embodiment 2

[0032] A kind of preparation method of 6,7-epoxy ligustilide, its steps are:

[0033] (1) Preparation of angelica extract: 1 kg of angelica medicinal material, crushed, passed through a No. 3 sieve, extracted by steam distillation, and 5.7 g of angelica volatile oil was obtained;

[0034] (2) Reaction: Add 40 ml of water-1,4-dioxane (10:90, v / v), 2 g of angelica volatile oil prepared in step (1) (42.1% ligustilide content, w / w) Add to a 100 ml round-bottomed flask one by one, and stir at room temperature for 5 minutes. Take 9 g of potassium hydrogen persulfate compound salt, slowly add it to the reaction system, stir at room temperature for 5 minutes, and then place it in a water bath at 100°C for reaction; the reaction process is monitored by liquid chromatography, and the peak area of ​​ligustilide in the reaction solution is The reaction is terminated when it is reduced by 85%;

[0035] (3) Separation: After the reaction, remove the insoluble matter by suction filtration...

Embodiment 3

[0037] A kind of preparation method of 6,7-epoxy ligustilide, its steps are:

[0038] Add 20 ml of water-methanol (5:95, v / v) and 0.5 g of crude ligustilide (content 80%, w / w) into a 50 ml round bottom flask in sequence, and stir at room temperature for 5 minutes; Slowly add 3 g of potassium bisulfate compound salt into the reaction system, stir at room temperature for 10 minutes, and then react in a water bath at 50°C; the reaction process is monitored by liquid chromatography, and the peak area of ​​ligustilide in the reaction solution is reduced by 80% After the reaction, the insoluble matter was removed by suction filtration, the filtrate was concentrated under reduced pressure at 40°C to remove the solvent, and the residue was separated by pressurized silica gel column chromatography (φ30 mm×200 mm), and the mobile phase was petroleum ether-ethyl acetate (6:1, v / v), fractions were collected at 20ml / part; the fractions were combined after UPLC detection, and the solvent wa...

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Abstract

The invention discloses a preparation method of 6,7-epoxy ligustilide, which belongs to the technical field of preparation of chemical components of traditional Chinese medicine. Potassium bisulfate compound salt is heated and reacted, and the reaction solution is treated and separated by silica gel column chromatography to obtain pure 6,7-epoxy ligustilide; the present invention provides a method for preparing 6,7-epoxy ligustilide A simple and easy method is obtained; moreover, a large amount of preparation of 6,7-epoxy ligustilide is realized, which provides convenience for further research on 6,7-epoxy ligustilide.

Description

technical field [0001] The invention relates to the technical field of preparation of chemical components of traditional Chinese medicines, in particular to a preparation method of 6,7-epoxy ligustilide. Background technique [0002] Ligustilide is a light yellow oily substance, belonging to natural phthalide compounds, mainly found in Umbelliferae plants, such as Chuanxiong ( Ligusticum chuanxiong Hort.), Angelica ( Angelica sinensis (Oliv.) Diels), Ligusticum ( Ligusticum sinense Oliv.) and other volatile oils or their fat-soluble extracts. [0003] Studies have shown that ligustilide can significantly improve the neurological function of rats with cerebral ischemia / reperfusion and reduce the volume of cerebral infarction; it can inhibit the expression level of inflammatory factors induced by lipopolysaccharide; it can inhibit the cognitive function caused by β-amyloid peptide. cognitive deficits, improve neuropathological symptoms; can enhance the endogenous antio...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D493/04
CPCC07D493/04
Inventor 陈雏吴燕李彬杜蕾蕾
Owner SICHUAN ACAD OF CHINESE MEDICINE SCI
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