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ChemicalBook CAS DataBase List Estra-4,9-diene-3,17-dione

Estra-4,9-diene-3,17-dione synthesis

5synthesis methods
-

Yield:5173-46-6 97%

Reaction Conditions:

with Jones reagent in acetone at 0;Jones Oxidation;

Steps:

1.11 Step 11: Preparation of Compound XII
The compound XI obtained in the tenth step (about 1.66 mmol) was dissolved in acetone (30 mL), the Jones reagent was slowly added at 0C until the color of the excess reagent did not disappear, and the end of the reaction was monitored by TLC. After 15 min, 2-propanol was added to consume excess Jones reagent. Saturated brine (40 mL) was added and the mixture was extracted with EtOAc (3 X 50 mL). The organic phases were combined and dried over anhydrous Na2SO4. After concentration under reduced pressure, the residue was purified by SiO 2 column chromatography (ΡΕ: ΕΑ=15:1) to give compound XII (435 mg, 97%, white solid).

References:

Sichuan University of Science and Engineering;Ma Xiaoyan CN108003210, 2018, A Location in patent:Paragraph 0060-0061

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