Method for preparing tripdiolide and 2-epitripdiolide

Abstract

The invention discloses a method for preparing tripdiolide and 2-epitripdiolide. Structures of triptonide, triptolide, tripdiolide and 2-epitripdiolide in common threewingnut root are quite similar, wherein tripdiolide and 2-epitripdiolide are a pair of chiral isomers and difficult to separate. When the four compounds are separated in the prior art, the separation depends on repeated silica-gel column chromatography, however, the repeated silica-gel column chromatography is high in solvent consumption, low in repeatability, just suitable for a small amount of separation in a laboratory and difficult to popularize in industrial production. The column chromatography which is only in use in the current industrial production is macroporous resin. According to the method, triptonide, triptolide, tripdiolide and 2-epitripdiolide can be separated and prepared without dependence on the repeated silica-gel column chromatography. With adoption of the HPLC method, tripdiolide and 2-epitripdiolidein the chiral isomers can be effectively separated on the basis of a conventional C18 chromatographic column, the cost is low, and the repeatability is high.

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...

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.

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