734-32-7Relevant articles and documents
Jacquesy et al.
, p. 4739 (1972)
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.
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.
