1,4-Dioxane → HCID 70638779, compound

Participants

Reaction Steps

A mixture of 3 g of 11β-hydroxy-17α,21-diacetoxy-6α-fluoro-pregn-4-ene-3,20-dione [compound 4, the product of Example 3] , 2.5 g of 2,3-dichloro-4,5-dicyanobenzoquinone, and 30 ml of dioxan was heated under reflux for 2 hours. The resulting dark colored suspension was cooled, filtered from dichloro-dicyanohydroquinone, and then evaporated to dryness. The residue so obtained was dissolved in chloroform and filtered through neutral alumina (50 g). The solvent was evaporated under reduced pressure. The residue crystallized from methanol as colorless prisms, m.p.: 235°-240°, λmax, 241 nm (ε= 14,200). The analytical sample of 11β-hydroxy-17α,21-diacetoxy-6α-fluoro-pregna-1,4-diene-3,20-dione (compound 5) was obtained by an additional recrystallization from methanol.

Provenance & Evidence