A kind of method for preparing triptolide

A triptolide ketone, one-in-ten-thousandth technology, applied in the chemical field, can solve the problems of poor reproducibility, solvent consumption, and difficulty in popularization, and achieve low cost and high reproducibility

Active Publication Date: 2019-04-02
HAIMEN BIWEI INTPROP SERVICE CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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 triptonide. Structures of the triptonide, triptolide, tripdiolide and 2-epitripdiolide existed in common caulis tripterygii wilfordii are close, whereinthe tripdiolide and the 2-epitripdiolide are a pair of chiral isomers with big separating difficulty. The four compounds are separated by depending on repeated silica column chromatography in the prior art, while repeated silica column chromatography consumes solvent, is poor in reproducibility, only suitable for less separation in experiments, and hard to popularize in industrial production. In current industrial production, only used column chromatography is a macroporous resin. The method provided by the invention can be used for separating and preparing the triptonide, the triptolide, thetripdiolide and the 2-epitripdiolide without depending on repeated silica column chromatography. The HPLC (Hight Performance Liquid Chromatography) method provided by the invention can be used for effectively separating the chiral isomers i.e. the tripdiolide and the 2-epitripdiolide based on a conventional C18 chromatographic column, and is low in cost and high 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 HAIMEN BIWEI INTPROP SERVICE CO LTD
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