Chlorosulfonic acid → HCID 13145955, compound

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Reaction Steps

Chlorosulfonic acid (2.0 ml) is added to methylene chloride (50 ml) containing 6β-fluoro-9α-hydroxyandrost-4-ene-3,17-dione (III, Example 2, 5.2 g) previously cooled to -20°. After 1.25 hr, the cold solution is quenched by adding slowly water (2 ml). The organic mixture is then washed with water, aqueous sodium carbonate, dried over sodium sulfate, and the organic solvent removed under reduced pressure to give the title compound. Rf (ethyl acetate/hexane, 1/1)=0.5; NMR (CDCl3) 0.9, 1.5, 5.1, 5.6 and 5.9 δ.

Provenance & Evidence