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Method for separating and preparing alpha-terthienyl, thianthrene and p-terphenyl

A technology for p-terphenyl and terphenyl thiophene, which is applied in the field of separation and preparation of α-terphenyl thiophene, thianthracene and p-terphenyl, and can solve the problem of not being able to obtain extremely high-purity monomers

Active Publication Date: 2011-08-31
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] It is reported in the existing literature that α-tertiary thiophene is prepared by Grignard reagent cross-coupling reaction, but the monomer with extremely high purity cannot be obtained, while the preparation method of countercurrent chromatographic separation can obtain high-purity monomer

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Select n-hexane-acetonitrile on the semi-preparative countercurrent chromatograph GS10AB to separate and purify the Falconium chrysanthemum extract (the raw material of Falconium chrysanthemum extracted from petroleum ether). Let stand to layer. After equilibrating for a period of time, separate the upper phase and the lower phase, take the lower phase as the stationary phase, and the upper phase as the mobile phase. A semi-preparative high-speed countercurrent chromatograph is used, equipped with NS-1007 pump, 20mL injection valve, polytetrafluoroethylene column with a column volume of 240mL, 8823A-UV ultraviolet detector, and Yokogawa 3057 portable recorder. Weigh 200 mg of the raw material of chrysanthemum chrysanthemum extracted from petroleum ether and dissolve it in a mixed solution of 5 mL of the upper phase and 5 mL of the lower phase for use. Before sample injection, fill the entire column with stationary phase, adjust the speed of the main engine to 800rpm, a...

Embodiment 2

[0013] Select n-heptane-dichloromethane-acetonitrile on the semi-preparative countercurrent chromatograph GS10A to separate and purify the extract of Falconium chrysanthemum (the raw material of Falconium chrysanthemum extracted from petroleum ether). In a liquid funnel, shake well and let stand to separate layers. After equilibrating for a period of time, separate the upper phase and the lower phase, take the lower phase as the stationary phase, and the upper phase as the mobile phase. A semi-preparative high-speed countercurrent chromatograph is used, equipped with NS-1007 pump, 20mL injection valve, polytetrafluoroethylene column with a column volume of 230mL, 8823A-UV ultraviolet detector, and Yokogawa 3057 portable recorder. Weigh 129.4 mg of the raw material of chrysanthemum chrysanthemum extracted from petroleum ether and dissolve it in a mixed solution of 5 mL upper phase and 5 mL lower phase for use. Before sample injection, fill the entire column with stationary pha...

Embodiment 3

[0015] Select n-pentane-dichloromethane-acetonitrile on the semi-preparative countercurrent chromatograph EMC-500A to separate and purify the extract of chrysanthemum chrysanthemum (raw material of chrysanthemum chrysanthemum extracted from petroleum ether). In a separatory funnel, shake well and let stand to separate layers. After equilibrating for a period of time, separate the upper phase and the lower phase, take the lower phase as the stationary phase, and the upper phase as the mobile phase. A semi-preparative high-speed countercurrent chromatograph is used, equipped with NS-1007 pump, 20mL injection valve, polytetrafluoroethylene column with a column volume of 500mL, 8823A-UV ultraviolet detector, and Yokogawa 3057 portable recorder. Weigh 400.1 mg of the raw material of chrysanthemum chrysanthemum extracted from petroleum ether and dissolve it in a mixed solution of 5 mL upper phase and 5 mL lower phase for use. Before sample injection, fill the entire column with the...

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Abstract

The invention relates to a method for separating and preparing high-purity monomers of alpha-terthienyl, thianthrene and p-terphenyl from plant flaveria bidentis extracts, obtained by petroleum ether refluxing, with high-speed countercurrent chromatography. In the method, the countercurrent chromatography is adopted to separate and prepare the high-purity alpha-terthienyl, thianthrene and p-terphenyl from the plant flaveria bidentis extracts, obtained by petroleum ether refluxing, a solvent comprises three components including petroleum ether or n-alkane, dichloromethane and acetonitrile or fatty alcohol in the volume ratio of 10:(0-3):(12-7); and the method is suitable for separation and preparation of the monomers of alpha-terthienyl, thianthrene and p-terphenyl through various models of countercurrent chromatographs, so that a large amount of crude products or synthetic mixtures can be directly fed, the purity of separated alpha-terthienyl is over 99%, and the purity of thianthrene and p-terphenyl can reach more than 90%.

Description

technical field [0001] The invention relates to a preparation and separation method for separating and preparing high-purity monomers α-terthiophene, thianthracene and p-terphenyl from the extract of alien invasive plant chrysanthemum chrysanthemum by high-speed countercurrent chromatography. Background technique [0002] Chrysanthemum [ Flaveria bidentis (L.) Kuntze] is the genus Chrysanthemum chrysanthemum (L.) Flaveria ) annual herb originating from South America. Chrysanthemum chrysanthemum plants are tall and dense, with amazing seed yield, strong reproductive ability and adaptability. It can invade various habitats such as farmland, roadside, and wasteland, and can inhibit the growth of other plants through allelopathy, thereby quickly occupying ecological niches. In addition to its origin, Chrysanthemum chrysanthemum is invasive in other countries and regions, posing a great threat to the ecological environment and agricultural production, and is a highly dangerou...

Claims

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Application Information

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IPC IPC(8): C07D333/06C07D339/08C07C15/14C07C7/12B01D15/08
Inventor 魏芸张凯
Owner BEIJING UNIV OF CHEM TECH
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