734-32-7Relevant academic research and scientific papers
Electrocatalytic oxidation production process and device for 19-normethyl-4-androstene-3, 17-diketone
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Paragraph 0028-0038, (2021/05/15)
The invention discloses an electrocatalytic oxidation production process and device for 19-normethyl-4-androstene-3, 17-diketone, and the process comprises the following steps: adding 19-hydroxymethyl-4-androstene-3, 17-diketone, nitroxide free radicals and a mixed solvent into an anode chamber to form an anode reaction solution, adding an alkaline buffer solution into a cathode chamber, dividing the electrolytic reaction tank into a left pole chamber and a right pole chamber by a cation exchange membrane so that the anode reaction liquid is driven to circularly flow between the anode chamber and the left pole chamber of the electrolytic reaction tank, and the alkaline buffer solution is driven to circularly flow between the cathode chamber and the right pole chamber of the electrolytic reaction tank, carrying out electrocatalytic oxidation reaction to generate an aldehyde intermediate 19-formaldehyde-4-androstene-3, 17-diketone, and then directly heating and stirring to react to obtain the product 19-normethyl-4-androstene-3, 17-diketone. Compared with the existing process for preparing 19-normethyl-4-androstene-3, 17-diketone which has the technical problems of high cost, serious environmental pollution, low yield and the like, the process has the advantages of low production cost, high target product yield, short production period and the like.
Method for preparing 19-desmethyl-4-androstene-3,17-diketone by using one-pot method
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Paragraph 0019, (2018/04/03)
The invention discloses a method for preparing 19-desmethyl-4-androstene-3,17-diketone by using a one-pot method. The method for preparing 19-desmethyl-4-androstene-3,17-diketone comprises the step oftaking a compound 1 as a starting raw material, carrying out hydrogenation and condensation reaction by using the one-pot method, thus obtaining a 19-desmethyl-4-androstene-3,17-diketone coarse product 3, wherein reaction formulas are as follows: as shown in the specification. According to the method, the high-purity 19-desmethyl-4-androstene-3,17-diketone coarse product can be obtained under a total mole yield of 92 percent or above, so that the method is low in cost, environmentally friendly and suitable for industrial production.
Synthesis process of paricalcitol
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Paragraph 0035; 0036, (2017/09/29)
The invention discloses a synthesis process of paricalcitol. The synthesis process of the paricalcitol comprises the steps of adopting nandrolone as a raw material, oxidizing, carrying out wittig reaction, carrying out hydroxy protection, brominating, rearranging, carrying out dehydrobromination, carrying out addition, oxidizing, reducing, carrying out hydroxy deprotection, and opening ring to obtain the paricalcitol. The paricalcitol is used for preventing and treating secondary hyperthyroidism.
Preparation method of 19-demethylation-4-androstenedione
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Paragraph 0007; 0010, (2017/08/30)
The invention discloses a preparation method of 19-demethylation-4-androstenedione and belongs to the technical field of medical intermediate processing. The preparation method comprises the following steps: (1) carrying out esterification reaction; (2) carrying out ketalation; (3) carrying out reduction reaction; (4) carrying out hydrolysis reaction; (5) carrying out esterification reaction; (6) carrying out addition reaction; (7) carrying out cyclization and hydrolysis reaction; (8) carrying out oxidation, dechloridation and ring-opening reaction; and (9) carrying out oxidation and decarboxylation reaction. The preparation method disclosed by the invention has the advantages that environmental pollution is small, usage amounts of a solvent and water are smaller, temperature sensitivity is low, control is easy, and yield is high; a chlorinating agent is adopted, so that reaction yield is increased; 1,3-dichloro-5,5-dimethylhydantoin is adopted, so that the reaction yield is further increased; and sodium hydrogen carbonate is adopted, so that final decarboxylic reaction yield is increased, and external standards and appearance of a product can be improved.
Preparation method of estra-4-ene-3,17-dione
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Paragraph 0042; 0043; 0047; 0048; 0052; 0053; 0057; 0058, (2017/08/29)
The invention provides a preparation method of estra-4-ene-3,17-dione. The method comprises the following steps: hydrogenation reaction: adding a first solvent and a palladium catalyst into a reaction container under the protection of nitrogen, stirring for 10 to 60 minutes, introducing hydrogen into the reaction container to replace the nitrogen, adding a raw material shown as a general formula I into the reaction container and stirring at the end of nitrogen replacement, heating to 10 to 60 DEG C, introducing hydrogen to react for 2 to 10 hours, separating the palladium catalyst out by using the nitrogen at the end of the reaction to obtain an intermediate solution of a compound shown as a general formula II, and keeping the intermediate solution for later use under the protection of the nitrogen; ring-closure reaction: concentrating the obtained intermediate solution to a viscous state under a normal pressure under the protection of the nitrogen, adding an acid-removing reagent into the viscous intermediate solution and stirring, reacting at the temperature of 60 to 100 DEG C for 0.5 to 5 hours, adding a second solvent into a solution obtained after the reaction, stirring for 10 to 30 minutes, dropwise adding reagent water, and cooling, filtering and drying to obtain the steroidal estrogen-4-ene-3,17-diketone shown as a general formula III, wherein a reaction route is shown in the description.
Method for preparing 19-nor-4-androstene-3,17-dione
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Paragraph 0024; 0027; 0030; 0033, (2017/08/28)
The invention discloses a method for preparing 19-nor-4-androstene-3,17-dione. The method comprises the following steps: taking a compound 1 as an initial raw material, carrying out a hydrolysis reaction, a hydrogenation reaction and condensation reaction so as to obtain 19-nor-4-androstene-3,17-dione, wherein the reaction formula is as shown in the specification. According to the method disclosed by the invention, a high-purity 19-nor-4-androstene-3,17-dione product is obtained at the total molar yield of 83% or higher, and the method is low in cost, green, environmental-friendly and suitable for industrial production.
New process for synthesizing steroid 3-one-4-ene
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Paragraph 0065; 0068; 0070, (2016/10/09)
The invention discloses a new process for synthesizing steroid 3-one-4-ene. The method comprises the steps: with steroid 3-hydroxy-5-ene as a starting material, in a nonprotic organic solvent, with air or oxygen as an oxidant and with a transition metal nitrate and a 2,2,6,6-tetramethylpiperidine-1-oxyl free radical or an analogue thereof as catalysts, oxidizing to obtain the steroid 3-one-4-ene. The method has the advantages of high yield, mild reaction conditions, easily controlled operation, low energy consumption, low cost, and safety; and the whole process is friendly to the environment, and is suitable for industrialization.
19-nor-4-androstene -3,17-dione method for the preparation of
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Paragraph 0037; 0045, (2016/11/28)
The invention provides a method for preparing 19- nor-4-androstene-3, 17-diketone. The preparation method comprises the following step: with a compound I as a raw material, carrying out a Grignard reaction, an oxidation and ring-closure reaction and a reduction and ring-closure reaction, and the reaction route is shown as follows. The starting raw material of the preparation method is relatively cheap, the product yield is high and the production cost can be saved. The formula is described in the description.
Imitation of phase i oxidative metabolism of anabolic steroids by titanium dioxide photocatalysis
Ruokolainen, Miina,Valkonen, Minna,Sikanen, Tiina,Kotiaho, Tapio,Kostiainen, Risto
, p. 45 - 55 (2015/01/09)
The aim of this study was to investigate the feasibility of titanium dioxide (TiO2) photocatalysis for oxidation of anabolic steroids and for imitation of their phase I metabolism. The photocatalytic reaction products of five anabolic steroids were compared to their phase I in vitro metabolites produced by human liver microsomes (HLM). The same main reaction types - hydroxylation, dehydrogenation and combination of these two - were observed both in TiO2 photocatalysis and in microsomal incubations. Several isomers of each product type were formed in both systems. Based on the same mass, retention time and similarity of the product ion spectra, many of the products observed in HLM reactions were also formed in TiO2 photocatalytic reactions. However, products characteristic to only either one of the systems were also formed. In conclusion, TiO2 photocatalysis is a rapid, simple and inexpensive method for imitation of phase I metabolism of anabolic steroids and production of metabolite standards.
Pd nanoparticles as catalysts for green and sustainable oxidation of functionalized alcohols in aqueous media
Mifsud, Maria,Parkhomenko, Ksenia V.,Arends, Isabel W.C.E.,Sheldon, Roger A.
experimental part, p. 1040 - 1044 (2010/04/02)
The previously described catalyst system for the aerobic oxidation of alcohols, comprising palladium(II) acetate in combination with neocuproine in a 1:1 mixture of water and a water-miscible cosolvent such as ethylene carbonate or dimethylsulfoxide, was shown to involve palladium nanoparticles as the active catalyst. The latter are formed in situ or can be preformed by reduction of the palladium-neocuproine complex with hydrogen and they are stabilized by both the neocuproine ligand and the cosolvent. This catalyst system was successfully used for the selective aerobic oxidation of the steroidal secondary alcohols, nandrolone and 5α-pregnan-3α-ol-20-one, to the corresponding ketones.
