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Process for preparing xanthones under a catalyst-free condition

A technology of xanthone and a process method is applied in the field of preparation of chemical raw materials, can solve problems such as environmental pollution, increase production cost and the like, and achieve the effects of reducing production cost, reducing production cost and simple process steps

Inactive Publication Date: 2021-01-05
HENAN UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the use of nitric acid catalyst not only increases the production cost, but also has environmental pollution problems.

Method used

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  • Process for preparing xanthones under a catalyst-free condition
  • Process for preparing xanthones under a catalyst-free condition
  • Process for preparing xanthones under a catalyst-free condition

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preparation example Construction

[0020] As a further optimization of the preparation method of xanthone in the present invention: the organic solvent is n-hexane, n-heptane, n-octane or cyclohexane.

[0021] As a further optimization of the preparation method of xanthone in the present invention: the amount of oxygen introduced is such that the pressure of oxygen in the reactor is 0.5-3 MPa.

[0022] As a further optimization of the preparation method of a xanthone of the present invention: the temperature during the reaction is 140-160°C.

[0023] As a further optimization of the preparation method of a xanthone of the present invention: the reaction time is 15-40h.

Embodiment 1

[0025] Take 2 mL of cyclohexane, 0.5 mmol of xanthene, and magnetons into a high-pressure reactor with a polytetrafluoroethylene liner, and then pass oxygen into the reactor until the pressure of oxygen in the reactor is 0.5 MPa , Then, seal the reaction kettle, put it into a heating tank with a temperature of 140° C., and carry out the reaction under magnetic stirring conditions for 20 h. After the reaction was completed, it was naturally cooled to room temperature. Afterwards, the internal standard quantitative analysis of the obtained product was carried out by using a gas chromatograph, and the yield of the xanthone product was measured to be 81%. Afterwards, the product is separated and purified by column chromatography to obtain the finished product of xanthone. use 1 H-NMR, 13 C-NMR confirms the structure of the product in the appendix figure 1 And attached figure 2 .

Embodiment 2

[0027] Take 2 mL of n-hexane, 0.5 mmol of xanthene, and magnetons into a high-pressure reactor with a polytetrafluoroethylene liner, and then pass oxygen into the reactor until the pressure of oxygen in the reactor is 0.5 MPa. Then, the reaction kettle was sealed and put into a heating tank with a temperature of 140° C., and reacted for 20 h under magnetic stirring conditions. After the reaction was completed, it was naturally cooled to room temperature, and then, the internal standard quantitative analysis of the obtained product was carried out by using a gas chromatograph, and the yield of the xanthone product was measured to be 73%. Afterwards, the product is separated and purified by column chromatography to obtain the finished product of xanthone.

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Abstract

The invention discloses a technological method for preparing xanthone under the catalyst-free condition. The method comprises the steps of dissolving xanthene into an organic solvent; introducing oxygen into the organic solvent; closing a reactor, and performing a reaction under high temperature, wherein the organic solvent is normal hexane or normal heptane or normal octane or cyclohexane, and the introduction amount of oxygen enables the pressure intensity of oxygen in the reactor to be 0.2-4 MPa, enables the reaction temperature to be 120-180 DEG C, and enables the reaction time to be 2-40h. Xanthene and oxygen are adopted as raw materials, xanthone is prepared under the condition that no catalyst or additive is added, waste in the production technology is reduced, the product is moreeasily purified, the product purity is remarkably improved, reaction solvents are recycled, and therefore the production cost is lowered, and environment contaminations are reduced.

Description

technical field [0001] The invention relates to the technical field of preparation of chemical raw materials, in particular to a process for preparing xanthone without a catalyst. Background technique [0002] Xanthones have significant pharmacological activity, and have pharmacological effects such as anti-depression, anti-virus, anti-tuberculosis, anti-cancer, and anti-hepatotoxicity ( synthetic chemistry , 2002, 10, 285-291), it is widely used in medicine, and is also used as a raw material for the synthesis of xanthan dyes, pesticides and other fine chemicals ( Dyes and Dyeing , 1982, 16-20). At present, the acquisition methods of xanthones in the prior art mainly contain the following types ( Journal of Zhoukou Normal University , 2012, 29 , 72-73): (1) Extracted from natural plants. For example, Cai Youqing's research group extracted and isolated xanthone derivatives ( Planta Medica ,1998, 64 , 64-70), the extract has antimalarial effects. Literature reports ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D311/86
CPCC07D311/86
Inventor 田欣哲建方方任运来王键吉程新强申振鹏赵哲
Owner HENAN UNIV OF SCI & TECH
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