ChemicalBook CAS DataBase List 10α-Pregna-5,7-diene-3,20-dione, cyclic bis(ethylene acetal) (8CI)

10α-Pregna-5,7-diene-3,20-dione, cyclic bis(ethylene acetal) (8CI) synthesis

4synthesis methods

Product Name:10α-Pregna-5,7-diene-3,20-dione, cyclic bis(ethylene acetal) (8CI)
CAS Number:32164-74-2
Molecular formula:C25H36O4
Molecular Weight:400.56

Pregn-5-ene-3,20-dione, 7-bromo-, cyclic 3,12-bis(1,2-ethanediyl acetal), (7α)-

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10α-Pregna-5,7-diene-3,20-dione, cyclic bis(ethylene acetal) (8CI)

32164-74-2
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Yield: 80%

Reaction Conditions:

with triethylamine at 120; for 2 h;Inert atmosphere;Reagent/catalyst;

Steps:

3-8
Put compound 4 into the reaction tank, add 3.5 L of organic base TEA, heat to 120 ° C ± 5 ° C under nitrogen protection, react at temperature for 2 h, recover about 2/3 of TEA under reduced pressure, and then add 3 L of acetonitrile / methanol = 1 / 1, cooled to below 60 ° C, added 500 ml of dioxane, cooled at -10 ° C ± 5 ° C, crystallized for 0.5 hours, filtered, and washed with 1.5L of water and 1.5L of acetone in order, dried, and dried at 40 ° C Overnight, pale yellow product Compound 5 was obtained in 80% yield.

References:

Guangxi Normal University;Pan Chengxue;Su Guifa;Yu Chenglong;Tan Jiangke;Li Yongyi;Yang Qian;Fang Shujun CN110818760, 2020, A Location in patent:Paragraph 0039; 0042-0049

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32164-74-2
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