4 results about "Eplerenone" patented technology

The application provides a method for synthesizing an eplerenone intermediate N-1 by one-pot method, and belongs to the technical field of organic synthesis. The method is characterized in that: the eplerenone intermediate N-4 is dissolved in dichloromethane, a potassium carbonate aqueous solution and dibromohydantoin are added to perform an opening ring reaction; after the reaction is completed, hydrochloric acid is directly added to perform a rearrangement reaction; then water is separated and methanol is added in the organic layer to perform an ozonation reaction; then sodium sulfite is added to perform a reduction reaction; then hydrochloric acid is added to perform a methyl esterification reaction, so as to obtain the eplerenone intermediate N-1 crude product, and finally the eplerenone intermediate N-1 fine product is obtained through refining. The method realizes the one-pot synthesis of the eplerenone intermediate N-1 from the eplerenone intermediate N-4 through the continuous reactions of opening ring, rearrangement, ozonation, reduction and methyl esterification, and can avoid column chromatography purification, so that the method becomes a green chemical process route with greatly reduced organic solvent consumption and wastewater.

The invention relates to the technical field of pharmaceutical chemicals, in particular to a refining method of an eplerenone intermediate. The method comprises the following steps: S1, dissolving: sequentially adding an eplerenone methyl ester crude product, an organic solvent and water into a reaction bottle, and stirring and heating to completely dissolve the eplerenone methyl ester crude product, the organic solvent and the water; s2, reaction: adding inorganic alkali into a dissolved reaction system, and stirring for full reaction at controlled temperature; s3, elutriation: cooling the system to room temperature, and slowly dropwise adding water to precipitate a solid product; s4, devitrification: cooling, devitrifying and fully stirring; s5, filtering and drying: filtering the system for solid-liquid separation, and drying to obtain an eplerenone methyl ester fine product. The eplerenone methyl ester refining method provided by the invention is high in product yield and low in cost, the adopted organic solvent is a common solvent and is low in toxicity, and the eplerenone methyl ester refining method has good industrial application value and is very suitable for large-scale industrial application.

The application discloses a purification method of eplerenone, which uses a mixture of alcohol and water as a recrystallization solvent. The technical scheme provided by the application can completely dissolve eplerenone, is friendly to the environment, has low toxicity, has high product yield and purity, has good impurity removal effect, has low dosage, and has a safer refining system, and is more suitable for industrialized and large-scale production.

The invention discloses a preparation method of eplerenone and an intermediate of eplerenone, and belongs to the technical field of chemical synthesis of medicines, and the preparation method comprises the following steps: by taking 9 alpha-hydroxy-4-androstene-3, 17-diketone which is low in price and easy to obtain as an initial raw material, firstly, constructing a delta9, 11-double bond with high selectivity through an acidic dehydration reaction; then, a gamma-lactone ring is efficiently constructed through 3-position carbonyl protection, 17-position propynylation and oxidative cyclization reaction, and an intermediate delta 9, 11-canrenone is obtained; further efficiently introducing carboxyl into the C7 site of the intermediate through a photocatalytic flow chemical technology, and finally preparing eplerenone through esterification and 9alpha, 11alpha-stereoselective epoxidation. The method is novel in route design, avoids the difficulty in selectivity and the use of toxic reagents in the traditional method, and is mild in condition in each step, high in yield, high in purity and suitable for industrial production.