Progesterone preparation method

Abstract

A progesterone preparation method comprises the following steps: adding dehydropregnenolone acetate, a palladium-carbon catalyst and ethyl acetate in a hydrogenation tank, wherein the hydrogenation reaction temperature is 35-45 DEG C, the hydrogenation pressure is 0.02-0.03 MPa, and the reaction time is 2.0-5.0 hours; adding an inorganic alkaline solution for hydrolysis reaction about 1.5-3.0 hours under the temperature of 25-30 DEG C; swashing by Mr Wolfowitz oxide water vapor so as to obtain progesterone crude product, obtaining progesterone pretreatment product sequentially through beating processing by 120# gasoline and suction filtration, dissolving the pretreatment product in ethanol, adding active carbon so as to obtain filter cakes sequentially through heating, reflowing, filtering while the solution is hot, filtrate cooling and re-filtering, and drying filter cakes to obtain the pure progesterone. According to the invention, the palladium-carbon catalyst and the vinegar naphtha solvent are adopted, the hydrogenation reaction can be carried out at near ordinary temperature, the progesterone yield is more than 72 percent, the purity is more than 99.5 percent, and both the energy consumption and manufacturing cost are reduced.

Description

technical field [0001] The invention relates to a synthesis method of progesterone, in particular to an industrial production method for synthesizing progesterone with dienolone acetate as a raw material. Background technique [0002] At present, the industrialized production process of progesterone is to use dienolone acetate as raw material, and undergo steps such as hydrogenation, hydrolysis, Woshi oxidation, pretreatment, and refining to obtain a fine product of progesterone. The hydrogenation reaction of dienolone acetate in the above process uses ethanol as a solvent and active nickel as a catalyst, and the hydrogenation reaction is carried out at a temperature of 34~36°C for 3.5 hours, and some manufacturers increase the hydrogenation temperature to 50±3°C Reaction for 5 hours, this kind of high-temperature hydrogenation reaction, the reaction time is long, and side reactions are prone to occur, so that the double bond at the 5th position in the dienolone acetate is a...

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to aim at the low yield of progesterone product existing in the preparation method of existing synthetic progesterone with dienolone acetate as raw material, the main impurity content is many, the purity is not high, the energy consumption and production cost are high Defects and deficiencies, provide an improved method for preparing progesterone with dienolone acetate as raw material; the hydrogenation reaction in this method is carried out at close to normal temperature, and its progesterone product yield and purity are higher, and the main impurity content Reduce, and can significantly reduce energy consumption and production costs