16-dehydropregnane dehydropregnenolone acetate compound and preparation method thereof

Abstract

The invention belongs to the technical field of organic photochemical synthesis, and discloses a 16-dehydropregnane dehydropregnenolone acetate compound and a preparation method, the 16-dehydropregnane dehydropregnenolone acetate compound comprises the following components by mass: 8-12 parts of pseudosteroid sapogenin, 35-50 parts of an organic solvent, 3-5 parts of a porphyrin photosensitizer, and 10-20 parts of acetic acid. According to the invention, the 16-dehydropregnane dehydropregnenolone acetate compound is prepared by a photosensitized oxidation method, so that the problem of environmental pollution is eliminated from the source. Meanwhile, a constant-temperature cooling device is arranged outside a photochemical reactor, constant-temperature cooling is carried out in the reaction, the reaction is cooled, a constant-temperature reaction environment is constructed, the water consumption can be reduced by the cooling method, and resources are saved. According to the invention, column chromatography separation is carried out after preparation, the operation is simple, the repeatability is good, the product purity is high, and the method is more suitable for industrial large-scale production.

Description

technical field [0001] The invention belongs to the technical field of organic photochemical synthesis, and in particular relates to a 16-dehydropregnone ketone alcohol acetate compound and a preparation method. Background technique [0002] At present, there are more than 300 kinds of steroid drugs, which are widely used in the fields of anti-inflammatory, anti-allergic, endocrine regulation, anti-aging and contraception. This type of drugs is the second largest drug family after antibiotics. 16-Dehydropregnenolone acetate (16-DPA) is the most important intermediate of steroid drugs, and more than 70% of steroid drugs are produced from it. 16-DPA is prepared from diosgenin through three steps of thermal cracking, oxidation and elimination. At present, the oxidation reaction of pseudodiosgenin uses chromic anhydride oxidation technology at home and abroad, but chromic anhydride is a highly toxic and highly corrosive oxidant, and the discharge of a large amount of chromium-c...

AI Technical Summary

Problems solved by technology

At present, the oxidation reaction of pseudodiosgenin uses chromic anhydride oxidation technology at home and abroad, but chromic anhydride is a highly toxic and highly corrosive oxidant, and the discharge of a large amount of chromium-containing solid waste and waste water accompanied by its use has caused serious environmental problems. Pollution

However, the current methods for the preparation of 16-dehydropregnone ketone alcohol acetates are complex in operation, serious in waste of resources and high in energy consumption.

[0003] Through the above analysis, the existing problems and defects of the prior art are: the current method for the preparation of 16-dehydropregnone dienone alcohol acetate compounds is complicated in operation, serious waste of resources and high energy consumption

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