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Synthesis method of hypericin

A synthetic method and technology of hypericin, applied in chemical instruments and methods, preparation of carbon-based compounds, preparation of organic compounds, etc., can solve the problem of less research on hypericin, separation and purification methods problem, to achieve the effect of simple synthesis route and low purification difficulty

Inactive Publication Date: 2018-11-23
上海凯伟化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, most of the existing methods in China stay on the extraction method of hypericin, and there are few studies on the methods of its separation and purification.

Method used

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  • Synthesis method of hypericin
  • Synthesis method of hypericin
  • Synthesis method of hypericin

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Embodiment Construction

[0016] The technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention. Apparently, the described embodiments are only some of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by persons of ordinary skill in the art without making creative efforts belong to the protection scope of the present invention.

[0017] The synthetic method step of hypericin is as follows:

[0018] (1) Dissolve JSTS-1 in 50 times the volume of acetic acid, add stannous chloride (dissolved in hydrochloric acid solution with a mass fraction of 15%) dropwise, the temperature is not higher than 130°C during the dropwise addition, and reflux at 120°C for 3h , cooled to room temperature, the solid precipitated, and dried by suction to obtain a yellow solid jsts-2, the route is as follows,

[0019]

[00...

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Abstract

The invention discloses a synthesis method of hypericin. JSTS-1 is dissolved into acetic acid; stannous chloride is dripped; heating reflux is performed; cooling is performed to room temperature; suction filtering and drying are performed; the material is dissolved into a mixed solvent of pyridine and piperidine; ferrous sulfate heptahydrate pyridine nitric oxide is added; replacement nitrogen gasprotection is performed; heating reaction is performed under light shielding; cooling and reduced pressure rotary drying are performed; diluted hydrochloric acid is added for stirring; suction filtering is performed; filter cake is washed by water to reach a neutral state; the filter cake is dissolved into methyl alcohol; silica gel is added; reduced pressure rotary drying is performed; column chromatography separation is performed; products are added into acetone; low-temperature illumination and vacuum rotary drying are performed; methyl alcohol is added; stirring heating is performed; then, active carbon is added; stirring is performed; suction filtering, mother liquid rotary drying, water addition stirring, and suction filtering are performed; water washing is performed until the mother liquid is clear; solid is scraped out; dichloromethane is added; stirring and suction filtering are performed; dichloromethane is washed until the mother liquid is clear; solid is dried; a target product is obtained. The synthesis method provided by the invention has the advantages that the synthesis route is simple; the purification difficulty is low; the total yield exceeds 60 percent; the synthesis method is suitable for industrialization.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a method for synthesizing hypericin. Background technique [0002] After several centuries of application and a large number of clinical trials, Hypericum Yee has confirmed its safety and effectiveness, which has attracted the attention of the medical community, and its demand is increasing day by day. From the perspective of application in Europe, both antidepressant preparations and external preparations are used in large dosages. According to statistics, there are 100 million patients in the world, and the dosage is extremely large. It can be seen that the untapped domestic and global markets have huge potential and are worthy of in-depth research and introduction to the market. Moreover, AIDS is rampant in the world, but there are not many treatment methods and drugs. The United States has developed a small amount of drugs, but monopolizes the patents. Chinese researchers ...

Claims

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Application Information

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IPC IPC(8): C07C46/00C07C50/36
CPCC07C45/65C07C46/00C07C50/36C07C49/747
Inventor 仇文俊
Owner 上海凯伟化工科技有限公司
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