Water → HCID 13190190, compound

Participants

Reaction Steps

1.5 g of 21-acetoxy-11β-hydroxy-16α,17α-methylenedioxy-1,4-pregnadiene-3,20-dione is dissolved in 510 ml of methanol and 111 ml of water and refluxed under agitation with 1.5 g of calcium carbonate for 24 hours. The calcium carbonate is removed by vacuum-filtering; the filtrate is concentrated to turbidity and poured on water. After the usual working-up process, the crude product is purified on 115 g of silica gel with a methylene chloride-acetone gradient (0-20% acetone), thus isolating 758 mg of 11β,21-dihydroxy-16α,17α-methylenedioxy-1,4-pregnadiene-3,20-dione, mp 220°-223° C. (decomposition).

Provenance & Evidence