A kind of ingenol and preparation method thereof

Abstract

The present invention provides ingenol and a preparation method therefor. The method comprises: by taking euphorbia lathyris seeds as raw materials, obtaining the ingenol through recovery, extraction, hydrolysis reaction and silica gel column chromatography. According to the ingenol and the preparation method therefor, types off solvents used in the whole preparation process are less; both an extraction solvent and an extracting solvent are methanol; the solvent can be reused, so that the production cost is reduced, and the production process is simplified; the hydrolysis reaction of an ingenol esterified compound is performed by use of a strong base; by virtue of this reaction, an esterified compound of the ingenol can be converted into the ingenol, so that the separation process is simplified; and the ingenol with purity higher than 98% can be acquired through silica gel column chromatography for separation, so that use of a high-pressure reversed phase chromatography system is avoided, and the separation conditions are simplified. By use of the preparation method provided by the present invention, industrial preparation of the ingenol can be achieved, the preparation yield is high, and the product purity is high.

Description

technical field [0001] The invention belongs to the technical field of separation and purification, and relates to ingenol and a preparation method thereof. Background technique [0002] Picato gel is currently the first and only preparation that can be used to treat actinic keratosis (AK). It has a certain effect on the early detection and treatment of skin cancer, and the preparation has a broad market prospect. The main component of Picato gel is ingenol methacrylate, which is mainly obtained from the synthesis of ingenol and angelic acid glycosides derived from the seeds of Capsicum sativa. The preparation of ingenol has been reported in related literatures, but the preparation scale is still in the laboratory stage, and the cost of industrial preparation is relatively high. [0003] For example, CN 103694096 A discloses a method for separating and purifying ingenol monomer. The invention uses Euphorbiaceae Euphorbiaceae traditional Chinese medicine Daffodil as raw mate...

AI Technical Summary

Problems solved by technology

Although this invention can realize the separation of ingenol, its steps are more complicated, the hydrolysis efficiency of step a is low, a large amount of strong alkali solution is needed and a large amount of highly volatile toxic solvent such as THF is used in the separation process, which is easy to harm the human body Cause damage, cause pollution to the environment, not suitable for industrial production, do not meet the requirements of green environmental protection, and in the purification process of products using gravity silica gel column chromatography, it needs to be eluted with gradient petroleum ether-ethyl acetate, and the solvent cannot be recovered Reuse, the cost is high, is not conducive to industrial production, and the product purity must reach more than 99%, it must be separated by silica gel column for many times, and it can be realized by multiple gradient elutions

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