13951-70-7Relevant articles and documents
Preparation method and application of 16, 17-dihydroxy steroid compound
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Paragraph 0166-0181, (2022/01/08)
The invention provides a preparation method and application of a 16, 17-dihydroxy steroid compound, and relates to the technical field of chemical synthesis. The method comprises the steps of: (a) reacting a compound shown as a formula I, lewis acid and an azole compound to obtain a compound shown as a formula II; and (b) reacting the compound as shown in the formula II, cyclic acyl peroxide and water, and then hydrolyzing under an alkaline condition to obtain a compound as shown in a formula III. Lewis acid and an azole compound are used in the dehydration reaction of the compound shown in the formula I, the operation is easy, the reaction conditions are mild, the energy cost is low, and the safety coefficient is high. The cyclic acyl peroxide is used in the oxidation reaction of the compound shown in the formula II, so that the method is good in atom economy, few in side reaction, free of excessive impurities, easy to implement and repeat, free of heavy metal participation, green, environment-friendly, safer and good in application prospect.
9-site dehalogenation method of steroid compound
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Paragraph 0020, (2020/05/01)
The invention discloses a 9-site dehalogenation method of a steroid compound. The method comprises the following steps: dissolving a 9-halogenated-11-hydroxyester steroid compound and a certain amountof an auxiliary agent into an organic solvent, heating to a certain temperature, dropwise adding tributyltin hydride, reacting for a period of time, detecting, carrying out reduced pressure concentration after the reaction is completed in order to remove part of the solvent, carrying out elution or adding the solvent for crystallization, filtering to obtain a target product 11-hydroxyester steroid compound, layering the obtained mother liquor, and recycling tributyltin oxide. Compared with a traditional steroid compound chromium salt dehalogenation process, the method of the invention has theadvantages of simplicity in operation, high safety, recycling of tributyltin oxide, three-waste pollution reduction and cost reduction.
Method for preparing 16 alpha-hydroxyprednisolone
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Paragraph 0011; 0030; 0034-0035; 0039-0040; 0044, (2020/07/02)
The invention discloses a method for preparing 16 alpha-hydroxyprednisolone, belonging to the technical field of medicine preparation and processing. According to the method, 21-hydroxypregna-1,4,9(11),16-tetraene-3,20-dione 21-acetate is used as an initial raw material and subjected to oxidation, bromo-hydroxylation, debromination and alcoholysis to prepare 16 alpha-hydroxyprednisolone. Accordingto the method for preparing 16 alpha-hydroxyprednisolone, generation of impurities in the reaction process can be effectively controlled by improving the defects of a traditional process, reaction process is mild, and an overall conversion rate is high; and the method disclosed by the invention has the advantages of low requirements on a reaction device, low operation cost, simplicity and convenience in operation, suitability for industrial production and higher market prospects.