A kind of method for preparing triptolide

A triptolide, one in ten thousand technology, applied in the chemical field, can solve the problems of poor reproducibility, solvent consumption, difficult to promote, etc., and achieve the effect of low cost and high repeatability

Active Publication Date: 2019-07-26
江西中德诚信科技有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This makes the separation of these four compounds very difficult
The prior art relies on repeated silica gel column chromatography when separating these four compounds. However, repeated silica gel column chromatography consumes solvent and has poor reproducibility. It is only suitable for a small amount of separation in the laboratory and is difficult to promote in industrial production.

Method used

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  • A kind of method for preparing triptolide
  • A kind of method for preparing triptolide
  • A kind of method for preparing triptolide

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Embodiment Construction

[0074] The following describes the substantive content of the present invention in detail in conjunction with the drawings and embodiments, but does not limit the protection scope of the present invention.

[0075] 1. Experimental materials

[0076] The dried roots of Tripterygium wilfordii were purchased from the Bozhou Chinese medicinal materials market, and were identified as the dried roots of Tripterygium wilfordii of the Euonymus family;

[0077] XDA-1B macroporous adsorption resin was purchased from Zhengzhou Qinshi Technology Co., Ltd.;

[0078] DM130 macroporous adsorption resin was purchased from Anhui Sanxing Resin Technology Co., Ltd.;

[0079] 95% ethanol, triethylamine, ethyl acetate, n-butanol, ammonia water and hydrochloric acid were purchased from Nanjing Chemical Reagent Co., Ltd.;

[0080] TBE-300C high-speed countercurrent chromatograph, Shanghai Tongtian Biotechnology Co., Ltd.

[0081] 2. Experimental method

[0082] A method for preparing triptolide ...

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Abstract

The invention discloses a method for preparing triptolide. Triptonide, triptolide, tripdiolide and 2-epitripdiolide in common threewingnut roots are of very approximate structures, tripdiolide and 2-epitripdiolide are a pair of chiral isomers with large separation difficulties. In the prior art, the four compounds are separated all through repeated silica-gel column chromatography, however, repeated silica-gel column chromatography consumes a great amount of solvents and is poor in reproducibility, only applicable to slight separation in laboratories, and hard to popularize in industrial production. In conventional industrial production, only a macroporous resin is available as column chromatography in service. By adopting the method disclosed by the invention, triptonide, triptolide, tripdiolide and 2-epitripdiolide can be separated and prepared without repeated silica-gel column chromatography. On the basis of a common C18 chromatographic column, the HPLC (High Performance Liquid Chromatography) method disclosed by the invention is capable of effectively separating chiral isomers, namely tripdiolide and 2-epitripdiolide, and is low in cost and good in repeatability.

Description

technical field [0001] The invention belongs to the field of chemistry, and relates to a preparation method and a separation and analysis method of known compounds, in particular to a method for preparing triptolide ketone, triptolide, triptolide and 2-epitriptolide and triptolide The HPLC separation and analysis method of B and 2-epitriptolide. Background technique [0002] Studies have found that four chemical components with very similar structures in Triptolide have excellent anti-tumor activity, namely: triptolide ketone, triptolide, triptolide and 2-epitriptolide. The structural formula is as follows: [0003] [0004] From the chemical structure, it can be found that the structures of these four compounds are very close, wherein triptolide and 2-epitriptolide are a pair of chiral isomers. This makes the separation of these four compounds very difficult. The prior art relies on repeated silica gel column chromatography when separating these four compounds. Howeve...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J73/00
CPCC07J73/003
Inventor 赖旭宇
Owner 江西中德诚信科技有限公司
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