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To a solution of 10.4 g of 3-O-methyl, 7α-propylestradiol 4 in 50 ml of methylene chloride were subsequently added 15 g. of powdered sodium acetate, 30 g of silicagel and 32 g of pyridinium chlorochromate. After stirring for 1 hr the oxidation was complete. Excess reagent was destroyed by addition of 1 ml of isopropanol, followed by 150 ml of hexane 10 min. later. All the precipitates were filtered over Celite, and the filtrate was concentrated to dryness. This provided 9.6 g of essentially pure ketone 5; Rf 0.54 (hept./ethyl acetate 7/3).

1. customExcess reagent was destroyed by addition of 1 ml of isopropanol
2. customfollowed by 150 ml of hexane 10 min.
3. filtrationAll the precipitates were filtered over Celite
4. concentrationthe filtrate was concentrated to dryness