Method for preparing triptonide

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

Active Publication Date: 2018-05-15
HAIMEN BIWEI INTPROP SERVICE CO LTD
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  • Abstract
  • Description
  • Claims
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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 ge

Method used

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  • Method for preparing triptonide
  • Method for preparing triptonide
  • Method for preparing triptonide

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Embodiment Construction

[0074] The following describes the essential content of the present invention in detail with reference to the drawings and embodiments, but the protection scope of the present invention is not limited thereto.

[0075] 1. Experimental materials

[0076] The dried roots of Tripterygium wilfordii were purchased from the Bozhou Traditional Chinese Medicine Market and were identified as the dried roots of Tripterygium wilfordii, a plant of the Euonymaceae family;

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

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

[0079] 95% ethanol, triethylamine, ethyl acetate, n-butanol, ammonia 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, tripto...

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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 method for preparing known compounds and a separation and analysis method, and in particular to a method for preparing triptolide, triptolide, triptoside and 2-epitriptoside, and tripterygium wilfordii HPLC separation and analysis method for B and 2-epitriptolide. Background technique [0002] Studies have found that four chemical components with very similar structures in Tripterygium wilfordii have excellent anti-tumor activity, namely: triptolide, triptolide, triptolide and 2-epitriptolide. The structural formula is as follows: [0003] [0004] It can be found from the chemical structure that the structures of these four compounds are very similar, among which triptolide and 2-epi-triptoside are a chiral isomer. This makes the separation of these four compounds very difficult. In the prior art, when separating these four compounds, all of them rely on repeated silica gel column chromatog...

Claims

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Application Information

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IPC IPC(8): C07J73/00
CPCC07J73/003
Inventor 赖旭宇
Owner HAIMEN BIWEI INTPROP SERVICE CO LTD
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