161511-08-6Relevant articles and documents
A 3-carbonyl-4-nitrogen mixed male steroid -17 β method for the preparation of carboxylic acid
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Paragraph 0034 - 0037, (2017/01/05)
The invention belongs to the field of organic chemistry and provides a preparation method for 3-carbonyl-4-aza-androstane-17 beta carboxylic acid. The method comprises the steps: (1) dissolving 3-carbonyl-4-aza-5-androstane-17 beta carboxylic acid in alkaline water, adding a palladium-carbon catalyst, and introducing hydrogen for performing hydrogenation; (2) filtering after the hydrogenation until the pH value of filtrate obtained by filtering is 3-5, filtering by a centrifugal machine to obtain a filter cake, washing the filter cake with water until eluate is neutral, and spinning-drying the filter cake so as to obtain a crude 3-carbonyl-4-aza-androstane-17 beta carboxylic acid product; and (3) pulping the crude 3-carbonyl-4-aza-androstane-17 beta carboxylic acid product with methyl alcohol, filtering by the centrifugal machine to obtain a filter cake, washing the filter cake with the methyl alcohol, spinning-drying, and drying so as to obtain a fine 3-carbonyl-4-aza-androstane-17 beta carboxylic acid product. Organic solvents are not used in the method provided by the invention, the economy and environment protection performances are realized, and the post-treatment is easy; the reaction is performed under an alkaline condition, the catalytic activity and the selectivity (the isomer ratio is low) of palladium-carbon are high, and the yield is high; by using the method, products with the relatively purity and relatively high yield can be obtained.